Ti-Cu-N hard nanocomposite films prepared by pulse biased arc ion plating

In this work, Ti-Cu-N hard nanocomposite films were deposited on high-speed-steel (HSS) substrates using a TiCu (88:12 at.%) single multi-component target by pulse biased arc ion plating. The influence of pulse bias voltages was examined with regard to elemental composition, structure, morphology and mechanical properties of the films. The Cu atomic content of Ti-Cu-N films was determined by Electron Probe Micro-Analyzer (EPMA). The structure and morphology were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Hardness and film/substrate adhesion were determined by nanoindenter and scratch test, respectively. The results showed that the content of Cu appeared to be in the range of 1.75-4.5 at.%, depending on pulse bias voltages. The films exhibit a preferred orientation TiN (1 1 1) texture when the substrate bias voltages were −100 V and −300 V, while the preferred orientation change to be a preferred orientation TiN (2 2 0) one when the substrate bias voltages increase to −600 V and −900 V. And no obvious sign of metal copper phase was observed. The SEM morphologies showed some macroparticles (MPs) on the surface of the films and the relative content of the MPs decreased significantly when the substrate bias voltages increased from −100 to −900 V. The maximum value (74 N) of the film/substrate adhesion of the films was obtained when the substrate bias voltage was −600 V with Cu content of 1.75 at.%. Hardness enhancement was observed, the value of the hardness increased firstly and reached a maximum value of 31.5 GPa, corresponding to Cu content of 1.75 at.%, and then it decreased when the substrate bias voltage changed from −100 to −900 V. The hardness enhancement was discussed related to the concept for the design of hard materials.     

Ti/TiN multilayer thin films deposited by pulse biased arc ion plating

In this work, the effect of modulation period (Λ) on Ti/TiN multilayer films deposited on high-speed-steel (HSS) substrates using pulse biased arc ion plating is reported. The crystallography structures and cross-sectional morphology of Ti/TiN multilayer films were characterized by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM), respectively. Their mechanical properties were determined via nanoindentation measurements, while the film/substrate adhesion via the scratch test. It was found that the highest hardness value reached 43 GPa for the modulation period of 54 nm, while the film/substrate adhesion also reached the highest value of 83 N. Furthermore, the hardness enhancement mechanism in the multilayer films is discussed.     

脉冲偏压电弧离子镀Cr-O薄膜结构及光学性能研究

采用脉冲偏压电弧离子镀技术在单晶硅基片及石英玻璃上制备了一系列均匀透明的Cr-O薄膜. 用场发射扫描电子显微镜、X射线衍射仪、X射线光电子谱、纳米压痕仪、紫外可见光分光光度计等方法对薄膜的表面形貌、膜厚、相结构、成分、元素的化学价态、硬度和光学性能等进行表征, 主要研究了偏压幅值对薄膜结构和性能的影响. 结果表明, 施加偏压可使薄膜的沉积质量明显提高, 其相结构由非晶态转变为晶体态, 并随着偏压幅值的增加, 由Cr₂O₃相向CrO相转变; 薄膜的硬度先增大后减小, 当偏压为-300 V时, 硬度达到最大值24.4 GPa; 薄膜具有良好的透光率, 最高可达72%; 当偏压为-200 V时, 薄膜的最大光学帯隙为1.88 eV.     

Deposition of TiSiN coatings by arc ion plating process

Titanium silicon nitride (TiSiN) thin films were deposited on tungsten cemented carbide tools by cathode arc ion plating (AIP) process using alloy TiSi targets. The effects of silicon addition and negative substrate bias on the development of the textures of films were studied systematically by varying the bias voltage from −20 to −200 V. The structural features of the films were investigated in detail using X-ray diffraction. The effect of the texture on such mechanical properties as hardness and adhesion of the films was also studied. A maximum hardness of 42 GPa was obtained at a DC substrate bias of −150 V. The characteristics of TiSiN thin films exhibited excellent adhesion of over 150 N. The cutting performance of end-mills and drillers was evaluated by milling and drilling of highly hardened material under high-speed cutting conditions. The results reveal that cutting tools with TiSiN coatings markedly outperformed those with TiN coatings, and the uncoated cutting tools. TiSiN coating increased the cutting lifetime to seven times that of the uncoated one.     

Synthesis of titanium nitride thin films deposited by a new shielded arc ion plating

Thin films of titanium nitride (TiN) were deposited on stainless steel substrates by a modified deposition technique, double-layered shielded arc ion plating with vicarious circular holes (DL-SAIP). The results show that the TiN film with the distance of 10 mm between the double-layered shield plates had the least droplets. The deposition rate of the films prepared with the new technique was more homogeneous than that of all the other shielded arc ion plating. The film/substrate adhesion and microhardness values of the TiN films were higher than 40 N and 18 GPa, respectively. Thus such TiN thin films can be expected in applications.     

反应离子镀光学薄膜的微观结构分析

用反应离子镀方法制备了ＴｉＯ２单层膜及ＴｉＯ２／ＳｉＯ２多层膜，用透射电子显微镜分别观察了由反应离子镀方法及传统蒸镀法二种不同工艺制得的ＴｉＯ２单层膜及ＴｉＯ２／ＳｉＯ２多层膜的断面结构，并对ＴｉＯ２单层膜进行了喇曼分析和卢瑟福背散射分析。     

Surface free energy of non-stick coatings deposited using closed field unbalanced magnetron sputter ion plating

Semiconductor IC packaging molding dies require wear resistance, corrosion resistance and non-sticking (with a low surface free energy). The molding releasing capability and performance are directly associated with the surface free energy between the coating and product material. The serious sticking problem reduces productivity and reliability. Depositing TiN, TiMoS, ZrN, CrC, CrN, NiCr, NiCrN, CrTiAlN and CrNiTiAlN coatings using closed field unbalanced magnetron sputter ion plating, and characterizing their surface free energy are the main object in developing a non-stick coating system for semiconductor IC molding tools. The contact angle of water, diiodomethane and ethylene glycol on the coated surfaces were measured at temperature in 20 °C using a Dataphysics OCA-20 contact angle analyzer. The surface free energy of the coatings and their components (dispersion and polar) were calculated using the Owens-Wendt geometric mean approach. The surface roughness was investigated by atomic force microscopy (AFM). The adhesion force of these coatings was measured using direct tensile pull-off test apparatus. The experimental results showed that NiCrN, CrN and NiCrTiAlN coatings outperformed TiN, ZrN, NiCr, CiTiAlN, CrC and TiMoS coatings in terms of non-sticking, and thus have the potential as working layers for injection molding industrial equipment, especially in semiconductor IC packaging molding applications.     

Low loss niobium oxides film deposited by ion beam sputter deposition

Thin films of niobium oxides are deposited by ion beam sputtering with a Kaufman-type ion source. The deposition rate is function of the oxygen partial pressure. There is an optimum oxygen pressure at 7 × 10^–5 Torr to deposite a stoichiometric film. The as-deposited films are amorphous. The optical parameters, including refractive index, extinction coefficient, and homogeneity, of the oxide films are influenced by post-baking temperature. The surface morphology measured by an atomic force microscope (AFM) shows that there is a certain range of optimum baking temperature which yields a smooth film and a good optical quality.     

脉冲偏压电弧离子镀CNx薄膜研究

用脉冲偏压电弧离子镀通过控制不同的氮流量在(100)单晶Si基片上制备了不同成分的CN_x薄膜.用光学显微镜,XPS,XRD,激光Raman和Nanoindenter等方法研究了薄膜的形貌、成分、结构和性能.结果表明,薄膜表面平整致密、氮含量随着氮流量的降低而降低、结构为非晶且为类金刚石薄膜;随着氮含量从18.9%降低到5.3%(摩尔百分比,全文同),薄膜的硬度和弹性模量单调增加而且增幅较大,其中硬度从15.0 GPa成倍增加到30.0 GPa;通过氮流量的调整能够敏感地改变薄膜中的sp³键的含量,是CN_x薄膜的硬度和弹性模量获得大幅度调整的本质原因. 关键词： x薄膜')" href="#">CN_x薄膜 脉冲偏压 电弧离子镀 硬度     

脉冲偏压电弧离子镀C-N-V薄膜的成分、结构与性能

用脉冲偏压电弧离子镀方法在硬质合金基体上制备了一系列不同成分的C-N-V薄膜.用X射线光电子能谱、激光Raman光谱、 X射线衍射(XRD)、透射电子显微镜(TEM)和纳米压痕等方法分别研究了薄膜的成分、结构与性能.Raman光谱,XRD和TEM结果表明,所制备的薄膜为在类金刚石(DLC)非晶基体上匹配有VN晶体的碳基复合薄膜.随V和N含量的增加,薄膜硬度与弹性模量先增加后下降,在N含量为204%,V含量为218%时薄膜硬度与弹性模量具有最大值,分别为368和5697 GPa,高于相同条件下制备的 关键词： C-N-V薄膜 类金刚石薄膜 纳米复合薄膜 电弧离子镀     

低压反应离子镀方法制备ITO透明导电膜

溅射镀膜方法是制备ITO透明导电膜最常用也是实验研究最多的方法。实验使用一种不同于溅射方法的另一种制备工艺—低压反应离子镀方法—制备ITO透明导电膜。实验对不同沉积速率和不同氧气流量对ITO透明导电膜的方块电阻以及光学透过率的影响进行了详细地分析,并综合比较得到了当沉积速率为0.5nm/s,氧气流量为24cm3/min时,在波长为550nm处,方块电阻为20Ω,λ=550nm透过率为90.8%的优质ITO透明导电膜。     

反应离子镀制备ITO膜

采用反应离子镀新工艺成功地在K9玻璃上制备了ITO(Indium Tin Oxide)透明导电膜,所制备的ITO膜在550～600nm波长范围内,典型的峰值透过率为89%,面电阻为34Ω/□。     

脉冲偏压电弧离子镀TiO2薄膜的力学与光学性能

用脉冲偏压电弧离子镀技术在玻璃基片上制备均匀透明的TiO₂薄膜.利用X射线衍射仪、原子力显微镜、扫描电子显微镜、紫外-可见透射光谱仪和纳米压痕仪等手段,对不同脉冲负偏压下合成薄膜的相结构、微观结构、表面形貌、力学和光学性能进行表征.结果表明，沉积态薄膜为非晶态.脉冲负偏压对薄膜性能有明显的影响.随偏压的增加，薄膜厚度、硬度和弹性模量均先增大后减小，前者峰值出现在100—200 V负偏压范围，后两者则在250—350V范围.300 V负偏压时薄膜硬度最高，薄膜达到原子级表面光滑度，均方 关键词： 2薄膜')" href="#">TiO₂薄膜 脉冲偏压电弧离子镀 硬度 折射率     

Structural and tribological properties of CrTiAlN coatings on Mg alloy by closed-field unbalanced magnetron sputtering ion plating

In this paper, a series of multi-layer hard coating system of CrTiAlN has been prepared by closed-field unbalanced magnetron sputtering ion plating (CFUBMSIP) technique in a gas mixture of Ar + N₂. The coatings were deposited onto AZ31 Mg alloy substrates. During deposition step, technological temperature and metallic atom concentration of coatings were controlled by adjusting the currents of different metal magnetron targets. The nitrogen level was varied by using the feedback control of plasma optical emission monitor (OEM). The structural, mechanical and tribological properties of coatings were characterized by means of X-ray photoelectron spectrometry, high-resolution transmission electron microscope, field emission scanning electron microscope (FESEM), micro-hardness tester, and scratch and ball-on-disc tester. The experimental results show that the N atomic concentration increases and the oxide on the top of coatings decreases; furthermore the modulation period and the friction coefficient decrease with the N₂ level increasing. The outstanding mechanical property can be acquired at medium N₂ level, and the CrTiAlN coatings on AZ31 Mg alloy substrates outperform the uncoated M42 high speed steel (HSS) and the uncoated 316 stainless steel (SS).     

Influences of nitrogen flow rate on the structures and properties of Ti and N co-doped diamond-like carbon films deposited by arc ion plating

In this paper, Ti-C-N nanocomposite films are deposited under different nitrogen flow rates by pulsed bias arc ion plating using Ti and graphite targets in the Ar/N2 mixture gas. The surface morphologies, compositions, microstructures, and mechanical properties of the Ti-C-N films are investigated systematically by field emission scanning electron mi- croscopy （FE-SEM）, x-ray photoelectron spectroscopy （XPS）, grazing incident x-ray diffraction （GIXRD）, Raman spectra, and nano-indentation. The results show that the nanocrystalline Ti（C,N） phase precipitates in the film from GIXRD and XPS analysis, and Raman spectra prove the presence of diamond-like carbon, indicating the formation of nanocomposite film with microstructures comprising nanocrystalline Ti（C,N） phase embedded into a diamond-like matrix. The nitrogen flow rate has a significant effect on the composition, structure, and properties of the film. The nano-hardness and elastic modulus first increase and then decrease as nitrogen flow rate increases, reaching a maximum of 34.3 GPa and 383.2 GPa, at a nitrogen flow rate of 90 sccm, respectively.     

离子束溅射制备低应力深紫外光学薄膜

采用离子束溅射制备了Al F3、Gd F3单层膜及193 nm减反和高反膜系,分别使用分光光度计、原子力显微镜和应力仪研究了薄膜的光学特性、微观结构以及残余应力。在优选的沉积参数下制备出消光系数分别为1.1×10~(-4)和3.0×10~(-4)的低损耗AlF_3和GdF_3薄膜,对应的折射率分别为1.43和1.67,193 nm减反膜系的透过率为99.6%,剩余反射几乎为零,而高反膜系的反射率为99.2%,透过率为0.1%。应力测量结果表明,AlF_3薄膜表现为张应力而GdF_3薄膜具有压应力,与沉积条件相关的低生长应力是AlF_3和GdF_3薄膜残余应力较小的主要原因,采用这两种材料制备的减反及高反膜系应力均低于50 MPa。针对平面和曲率半径为240 mm的凸面元件,通过设计修正挡板,250 mm口径膜厚均匀性均优于97%。为亚纳米精度的平面元件镀制193 nm减反膜系,镀膜后RMS由0.177 nm变为0.219 nm。     

Structural and mechanical properties of compositionally gradient CrNx coatings prepared by arc ion plating

Compositionally gradient CrN_x coatings were fabricated using arc ion plating by gradually increasing N₂ flow rate during the deposition process. The effect of substrate bias, ranging from 0 to −250 V, on film microstructure and mechanical properties were systematically investigated with XRD, SEM, HRTEM, nanoindentation, adhesion and wear tests. The results show that substrate bias has an important influence on film microstructure and mechanical properties of gradient CrN_x coatings. The coatings mainly crystallized in the mixture of hexagonal Cr₂N, bcc Cr and fcc rock-salt CrN phases. N₂ flow rate change during deposition results in phase changes in order of Cr, Cr + Cr₂N, Cr₂N, Cr₂N + CrN, and CrN, respectively, along thickness direction. Phase fraction and preferred orientation in CrN_x coatings vary with substrate bias, exerting an effective influence on film hardness. With the increasing of bias, film microstructure evolves from an apparent columnar structure to a highly dense one. The maximum hardness of 39.1 GPa was obtained for the coatings deposited at a bias of −50 V with a friction coefficient of 0.55. It was also found that adhesion property and wear resistance of gradient CrN_x coatings were better than that of homogeneous CrN coatings.     

Surface modification of hard alloy by Y ion implantation under different atmosphere

To enhance the properties of hard alloy, rare-earth metal yttrium (Y) was implanted into its surface by using Metal Vapor Vacuum Arc (MEVVA) source implantor. The experiments were finished under different vacuum conditions with/without aerating nitrogen in the chamber. The metallograph and phase formation of sample were characterized and analyzed with metallurgical microscope and X-ray diffraction. The results show that there exist new phases of C, YC₂, Y₂O₃, and WN in the sample surface. Moreover, it can be found that the performances of sample surface (such as microhardness, friction coefficient and corrosion resistance) are evidently improved, and that nitrogen atmosphere plays a very important role in farther promoting these performances. The surface modification of hard alloy is not only affected by the implantation itself, but also related to the microstructure transformation, which can be partly induced by the atmosphere.     

离子束辅助工艺中APS源偏转电压对HfO2薄膜性能的影响

基于Leybold APS1104镀膜系统,采用离子束辅助反应沉积技术,以金属Hf粒为初始镀膜材料,APS源偏转电压为50~140 V范围内,在［100］单晶硅片和紫外石英（JGS1）基板上制备了HfO2单层膜。分别利用Lambda 900分光光度计、X射线光电子能谱仪、X射线衍射仪以及原子力显微镜对HfO2薄膜的光谱性能、表面及纵向化学成分、晶相结构以及表面粗糙度进行了分析。结果表明：当APS源偏转电压在120~140 V及50~90 V两个范围内变化时,HfO2薄膜的紫外短波光学损耗随着偏转电压的降低而减小,而为110~90 V时紫外短波光学损耗对偏转电压的变化不敏感;偏转电压在50~140 V的范围内时,制备的HfO2薄膜表面及纵向化学成分无明显变化;当偏转电压为100 V时,HfO2薄膜晶粒尺寸及表面粗糙度分别达到最大值26.2 nm及5.79 nm,其后,随着偏转电压的降低,二者均逐渐减小。     

Analysis of the composition of Ti-based thin films deposited on silicon by means of self-ion assisted deposition

The composition of Ti-based thin films deposited on silicon using a self-ion assisted deposition (SIAD) method was investigated by utilising the Rutherford backscattering spectrometry technique and RUMP simulation code. The hydrogen affinity of the coatings produced by means of SIAD was investigated using the ¹H(¹⁵N, αγ)¹²C nuclear resonance reaction. The titanium–based films on silicon were found to have a high content of oxygen, carbon, hydrogen and substantial concentration of the substrate. Near 10% H content enrichment was found at the surface of coatings but no hydrogen enrichment at the coating–substrate interfaces was observed.