离子束流密度和基底温度对TiN纳米薄膜性能的影响

采用低能离子束辅助沉积技术在Si片上制备了TiN纳米薄膜.考察了离子束流密度和基底温度对薄膜性能的影响.研究表明:随着离子束流密度的增大,TiN薄膜的纳米硬度上升,膜基结合力变化不大,薄膜的耐磨性获得了很大改善;制膜时的基底温度升高,薄膜的硬度也会上升,但膜基结合力下降,摩擦系数增大,薄膜的耐磨性下降.     

脉冲偏压对离子束辅助电弧离子镀TiN/Cu纳米复合膜结构及硬度的影响

采用离子束辅助电弧离子镀技术在高速钢基体上制备TiN/Cu纳米复合薄膜,考察了基体脉冲负偏压对薄膜成分、结构及硬度的影响。用X射线光电子谱、X射线衍射、扫描电镜、透射电镜和纳米压痕等方法分别测试了薄膜的化学成分、结构、表面形貌、硬度以及弹性模量。结果表明,在氮离子束的轰击作用下,随着脉冲偏压幅值从-100 V增加到-900 V时,薄膜中Cu含量先增加而后略有降低,在1.05%~2.50%(原子比)范围内变化。同时,脉冲偏压对薄膜的结构也有明显影响,在-100 V出现TiN(111)择优取向,当基体偏压增加到-300 V以上时,择优取向改变为TiN(220)择优。薄膜的Cu2p峰均对应纯金属Cu,薄膜的晶粒尺寸约在11~17 nm范围内变化。硬度和弹性模量随着偏压幅值增加而增大,当偏压为-900 V时,薄膜硬度和弹性模量达到最大值,分别为29.92 GPa,476 GPa,对应的铜含量为1.91%。     

基于TiN涂层/玻璃基体的热压印模板的制备与性能

对于热压印光刻而言,制备具有精确几何结构、良好耐磨损性能以及长使用寿命模板至关重要.在分析现有Si或SiO2模板使用性能基础上,提出了在TiN涂层/玻璃基体上制备热压印模板.首先采用直流磁过滤电弧在玻璃上沉积TiN薄膜,然后,通过聚焦离子束在薄膜上加工出最小线宽71nm的栅型结构,最后,使用所加工的模板,进行热压印实验,获得了良好的压印结果.实验结果表明,TiN作为模板材料可以获得高保真度的纳米图案,并且由于TiN比Si或SiO2具有更高硬度和强度,玻璃基体也具有很好的机械性能,由TiN/玻璃系统制备的压印模板的机械性能和使用寿命较之Si或SiO2基模板得到很大提高.     

不同能量离子束辅助沉积对形成氮化钛薄膜性能的影响

用不同能量离子束辅助沉积方法在医用不锈钢317L和Si(100)基底上沉积TiN薄膜。通过X射线光电子能谱(XPS)、X射线衍射(XRD)和俄歇电子能谱(AES)分析研究了薄膜的结构特征;测试了薄膜与基底的附着力和耐磨性;用电化学腐蚀的方法检测了薄膜在Hank’s模拟体液中的耐腐蚀性能;最后采用成纤堆细胞、骨髓细胞体外培养试验考察了生长于不同薄膜表面的细胞粘附、增殖、展布情况及细胞的形态。研究结果表明：用高、低能氮离子兼用的IBAD方法制备的TiN多晶薄膜比只用高能或低能沉积的薄膜具有更强的附着力和耐磨性,在Hank’s模拟体液中显示出更强的抗腐蚀能力,并在细胞体外培养中显示出良好的细胞相容性。     

离子束增强沉积TiN薄膜的研究

利用多功能离子束增强沉积设备，采用三种不同工艺方法制备TiN薄膜，并对制备的TiN薄膜进行了AES，XPS，XRD，RBS和TEM等分析。结果表明：所制备的薄膜都有很好均匀性，TiN薄膜处在压应力状态；在溅射沉积的同时，在0～20keV范围内，N 和Ar 离子的轰击使得TiN薄膜的生长呈现不同择优取向；随着N 离子轰击能量的增加，制备的TiN薄膜的晶粒增大。     

新型铁电薄膜底电极TiN的结构与电性能研究

自制了导电的TiN薄膜底电极,并在其上制备了铁电钽酸锂薄膜,测试了TiN薄膜电阻随热处理温度变化的关系,以及TiN底电极上钽酸锂薄膜的介电和漏电特性.实验结果表明,当热处理温度低于700℃时,TiN薄膜的电阻率小于0.004QΩ·cm,具有良好的导电性,可用作钽酸锂薄膜底电极;TiN底电极上钽酸锂薄膜的漏电电流大于Pt衬底上钽酸锂薄膜的漏电电流;N2气氛下在TiN底电极上结晶的钽酸锂薄膜的介电损耗远大于O2气氛下结晶的钽酸锂薄膜的介电损耗;氧缺位是TiN底电极上钽酸锂薄膜介电损耗大和漏电大的主要原因.     

磁控溅射TiAIN和WTiN薄膜的制备与摩擦性能研究

采用双靶反应磁控溅射的方法在40Cr基体上制备了TiAlN薄膜和WTiN薄膜。用XRD,SEM,AFM等检测手段对薄膜的表面状态及结构等进行了表征,采用UMT-3型多功能摩擦试验机,在室温、大气环境、无润滑的条件下对TiAlN和WTiN薄膜的摩擦性能进行了评价。实验结果表明:TiAlN薄膜出现了两种硬质相TiN与TiAlN共存的物相结构,而WTiN薄膜出现了TiN0.6O0.4,TiN,W2N,WN等多种物相结构;制备的TiAlN、WTiN薄膜表面晶粒均匀细小,生长均以粒状结构为主;摩擦实验数据表明制备的TiAlN和WTiN薄膜均拥有良好的摩擦性能。     

反应溅射TiN纳米晶薄膜的结构特征和耐蚀性

利用直流反应溅射技术在不锈钢和硅基体上沉积了TiN纳米晶薄膜,采用场发射扫描电镜(FESEM)、X射线衍射(XRD)和电化学阻抗谱(EIS)技术研究了薄膜的表面形貌、相结构和耐蚀性与偏压的关系。结果表明,TiN薄膜的表面结构明显取决于所施加的偏压,适当提高偏压有利于获得细小、均匀、致密和光滑的膜层。XRD分析发现,TiN薄膜为面心立方结构,其择优取向为(111)面。实验显示,对应0V和-35V偏压的薄膜为欠化学计量比的,而偏压增加至-70V和-105V时的薄膜为化学计量比的TiN。EIS结果表明,较高偏压下的TiN薄膜几乎在整个频率范围内均表现为容抗特征,其阻抗模值明显高于低偏压下的膜层,这主要与较高偏压下的薄膜具有相对致密的微结构有关。较低偏压的TiN薄膜因结构缺陷较多其耐蚀性低于基体不锈钢。EIS所揭示的薄膜结构特征与FESEM观测结果一致。可见,减少穿膜针孔等结构缺陷有利于改善反应溅射TiN纳米晶薄膜耐蚀性。     

大面积PET基中频反应磁控溅射沉积TiN隔热薄膜实验研究

本文讨论在柔性基材PET上沉积氮化钛(TiN)阳光控制膜——作为隔热薄膜.“隔热”是指对红外光区的有效阻隔.氮化钛(TiN)薄膜具有光谱选择透过性,因此可以作为阳光控制薄膜使用.实验采用中频孪生靶磁控溅射实验装置,在等离子体辐射监视系统( PEM)的控制下,在大面积PET柔性基材上沉积TiN隔热薄膜.实验主要研究了制备不同透光率的PET基TiN隔热膜并观察薄膜表面状况;对沉积的TiN薄膜用分光光度仪进行光谱透过率分析并计算各种透过率薄膜的光学性能参数,比较不同透过率的隔热效果;为了对该隔热薄膜的化学稳定性进行分析,还做了耐酸碱性测试.通过本实验为以后的大规模工业产业化发展奠定良好的基础.     

不同测试条件下TiN薄膜的摩擦学特性研究

采用电弧离子镀技术在45#钢衬底表面沉积了TiN薄膜.用显微硬度计测试了薄膜的硬度,用球一盘式摩擦磨损试验机评价了在不同测试条件下(干摩擦,水润滑,油润滑)TiN薄膜的摩擦学性能,用表面轮廓仪测试了磨痕处的磨痕轮廓,用配有能谱仪(EDS)的扫描电镜(SEM)观察和测试了磨痕形貌和磨痕处主要化学元素组成.结果表明,相对于干摩擦,水润滑和油润滑条件下,TiN薄膜的摩擦系数和磨痕深度都有明显降低的趋势.干摩擦条件下,薄膜表现为磨粒磨损和氧化磨损;水润滑条件下,薄膜表现为疲劳磨损,水对薄膜起到边界润滑作用;油润滑条件下,薄膜几乎无磨损,油起到流体润滑作用.     

结构调制超硬Ti/TiN纳米多层膜的制备及其尺寸效应

使用多弧离子镀技术在高速钢基体上制备了调制周期为5~40 nm的Ti/TiN纳米多层膜,用扫描电子显微镜(SEM)、X射线能谱仪(EDS)、X射线衍射仪(XRD)、纳米压痕仪和划痕仪等手段表征薄膜的微观结构和性能,研究了调制周期对Ti/TiN纳米多层膜性能的影响,并讨论了在小调制周期条件下Ti/TiN纳米多层膜的超硬效应和多弧离子镀技术对纳米多层膜硬度的强化作用。结果表明,与单层TiN相比,本文制备的Ti/TiN纳米多层膜分层情况良好,薄膜均匀致密,没有明显的柱状晶结构,TiN以面心立方结构沿(111)方向择优生长。随着调制周期的减小薄膜的硬度呈现先增大后减小的趋势,并在调制周期为7.5 nm时具有最大的硬度42.9 GPa和H/E值。这表明,Ti/TiN在具有最大硬度的同时仍然具有良好的耐磨性和韧性。Ti/TiN纳米多层膜的附着力均比单层TiN薄膜的附着力高,调制周期为7.5 nm时多层膜的附着力为(58±0.9) N。     

Effect of bias voltage on microstructure and mechanical properties of nanocrystalline TiN films deposited by reactive magnetron sputtering

Nanocrystalline TiN films deposited under various bias voltages have been prepared by a reactive magnetron sputtering. The effect of bias voltage on the microstructural morphologies of the TiN films was characterized by FE-SEM and AFM. The texture of the TiN films was characterized by XRD. It is also observed that the crystallite size decreases with increasing bias voltages. However, rms roughness increases with increasing bias voltages. The changes in roughness and crystallite size in the TiN thin films are due to one or a combination of factors such as resputtering, ion bombardment, surface diffusivity and adatom mobility; the influence of each factor depends on the processing conditions.     

Effects of nitrogen ion implantation and implantation energy on surface properties and adhesion strength of TiN films deposited on aluminum by magnetron sputtering

The performance of tribological coatings depends greatly on the adhesion strength between the coatings and substrates. In this work, we investigated the influence of the ion implantation energy of nitrogen on the adhesion and surface properties of TiN deposited on aluminum substrate. Aluminum samples were implanted with 15 keV, 30 keV and 40 keV nitrogen ions before TiN films were deposited using magnetron sputtering in a custom-designed multi-functional ion implanter. The adhesion properties of the implanted TiN films were assessed using nano-scratch tests and were observed to vary with the nitrogen ion implantation energy. Our frictional test results show that an appropriate ion implantation energy and dose can improve the frictional behavior of TiN films deposited on aluminum.     

Microstructural characteristics and mechanical properties of magnetron sputtered nanocrystalline TiN films on glass substrate

Nanocrystalline TiN thin films were deposited on glass substrate by d.c. magnetron sputtering. The microstructural characteristics of the thin films were characterized by XRD, FE-SEM and AFM. XRD analysis of the thin films, with increasing thickness, showed the (200) preferred orientation up to 1·26 μm thickness and then it transformed into (220) and (200) peaks with further increase in thickness up to 2·83 μm. The variation in preferred orientation was due to the competition between surface energy and strain energy during film growth. The deposited films were found to be very dense nanocrystalline film with less porosity as evident from their FE-SEM and AFM images. The surface roughness of the TiN films has increased slightly with the film thickness as observed from its AFM images. The mechanical properties of TiN films such as hardness and modulus of elasticity (E) were investigated by nanoindentation technique. The hardness of TiN thin film was found to be thickness dependent. The highest hardness value (24 GPa) was observed for the TiN thin films with less positive micro strain.     

室温磁控溅射制备(Ti,Zr)N薄膜及其性能研究

采用直流反应磁控溅射工艺,在载波片和Al基材上制备出金黄色的(Ti,Zr)N薄膜.(Ti,Zr)N薄膜具有比TiN薄膜更高的硬度和更强的耐腐蚀性能.用XRD衍射方法和扫描隧道显微镜对薄膜的晶体结构、微观表面形貌和电子结构进行了测试分析.XRD结果表明,(Ti,Zr)N薄膜为多晶态,存在TiN和ZrN两种分离相;从表面形貌可知,薄膜表面平整,晶粒排列致密且无连接松散的大颗粒;STS谱表明,Zr掺杂后,禁带宽度仍为1.64eV,但在禁带内增加了新能级,新能级的宽度分别为0.33eV和0.42eV,这也正是掺杂Zr后,薄膜仍呈现金黄色的主要原因.     

离子束增强沉积制备TiB_2薄膜及其性能研究

用离子束增强沉积法（IBED）在硅及铜基体上沉积了TiB2薄膜，研究了轰击离子束能量和束流对薄膜的微结构及力学性能的影响。用俄歇电子谱（AES）分析了膜的成分及其界面状况，用X射线衍射（XRD）研究了膜的微结构，并测定了膜的硬度及进行了膜的高温氧化试验。结果指出：（1）离子束轰击使薄膜晶化，从而影响到膜的硬度及抗高温氧化性能；（2）离子束增强沉积的二硼化钛薄膜是一种耐高温氧化的高硬膜。     

氮离子束轰击对电弧离子镀TiN膜层的作用

电弧离子镀膜层中"大颗粒"的存在,降低了膜层质量,限制了其进一步应用.采用俄罗斯UVN 0.5D2I离子束辅助沉积电弧离子镀设备,对高速钢W18Cr4V上沉积的TiN膜层进行了氮离子束轰击.结果表明:TiN膜层表面"大颗粒"完全消失,凹坑浅而平整,粗糙度降低.膜层中较软的Ti和Ti2N向TiN转变,TiN(111)取向逐渐减弱,而(200)取向逐渐增强.膜层的显微硬度由原来的1 980 HV1N升高到2 310HV1N.     

Effects of nitrogen partial pressure on microstructure,morphology and N/Ti ratio of TiN films deposited by reactive magnetron sputtering

Abstract

TiN films were deposited on Si(111) substrates at different nitrogen partial pressures with reactive magnetron sputtering. The crystal structure and preferred growth orientation of the films were determined using X-ray diffraction (XRD) analysis. Their morphology and composition were analysed using field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). It is found that with the increase in nitrogen partial pressure, the growth of TiN films varies from the {111} preferred orientation to the {100} preferred orientation and the deposition rate of TiN films decreases. When the {111} preferred orientation is presented, TiN films reveal a kind of surface morphology of triangular pyramid with right angles; while the {100} orientation is dominant, TiN films characterise another kind of domelike surface morphology. Furthermore, the N/Ti ratio of the TiN films first increases, then decreases and increases again as nitrogen partial pressure enlarges.     

轰击能量对离子束增强沉积Cr-N薄膜微观结构和硬度的影响

采用离子束增强沉积（IBED）技术，在不同能量氮离子的辅助轰击下制备了Cr－N薄膜；通过SEM观察、XRD分析和显微硬度测定，发现离子轰击能量对Cr－N薄膜的表面形貌、相组成和硬度有显著的影响：随着能量的升高，膜表面形貌由岛形颗粒状转变成蜂窝状；一定能量轰击下获得的Cr2N和CrN混相结构有最高的薄膜硬度；高达16keV的氮离子轰击可诱发非晶化的出现，并对膜有一定的强化作用。在此基础上探讨了离子轰击能量对合成Cr－N薄膜结构与性能的影响效应。