氮气辅助氙离子束增强沉积TiN薄膜及其机械性能

本文提出一个合成TiN硬质薄膜的新方法,在氮气氛中,电子束蒸发沉积Ti的同时,用40keV的氙离子束对其进行轰击而合成TiN薄膜,该方法优于PVD和CVD之处在于合成温度低,薄膜与基体结合力强,其临界载荷达4.2kg,Knoop硬度达2200kg/mm~2,具有良好的耐磨损性能,报道了所合成的TiN薄膜在工业上应用的一些结果。     

离子束增强沉积TiN薄膜界面结合强度的研究

采用划痕法测定了离子束增强沉积ＴｉＮ薄膜的界面结合力。结果表明，由于在离子束增强沉积过程中ＴｉＮ薄膜和基体之间生成一层厚约３０～４０ｎｍ的过渡层，从而大大改善了涂层的界面结合强度，其临界载荷可达１４０Ｎ，为一般ＰＶＤ和ＣＶＤ方法所生成的ＴｉＮ膜的３～４倍，并且发现它并不随膜厚的增加而变化。     

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 利用磁过滤阴极电弧镀分别在硬质合金和高速钢基体上沉积厚度约2～3μm的TiN薄膜,并用MEVVA源离子注入装置对TiN薄膜注入金属离子V+和Nb+。应用北京同步辐射装置（BSRF）的同步辐射光源,采用掠入射X射线衍射（GIXRD）的方法对TiN薄膜表面离子注入层的微观结构进行了分析研究。结果表明：未经过离子注入的TiN薄膜均存在特定方向的择优取向,而较小剂量(1×10ˇ17ions/cm2)的离子注入可以使晶粒细化、择优取向减弱或改变;当离子注入的剂量达到5×10ˇ17ions/cm2时,TiN薄膜表面离子注入层被非晶化。结合透射电镜的研究结果,观察到TiN薄膜表面非晶层的厚度约为50～100nm,并简要地讨论了离子注入过程对微观结构的影响机制。     

TiN薄膜的合成及其性能研究

用电子束蒸发沉积钛和40keV氮离子束轰击交替进行的办法合成了TiN薄膜。用RBS,AES,TEM,XPS,和X射线衍射研究TiN薄膜的组分和结构表明:用离子束增强沉积制备的TiN薄膜主要由TiN相构成;晶粒大小为30—40um,无择优取向;而非离子束轰击沉积的薄膜则是无定形的;用离子束增强沉积制备的TiN薄膜,其氧含量明显小于无离子束轰击薄膜的值;在TiN薄膜和衬底之间存在一个界面混合区,厚度为40um左右。机械性能测试表明,TiN薄膜具有高的显微硬度,低的摩擦系数。     

Influence of Si content and growth condition on the microstructure and mechanical properties of Ti-Si-N nanocomposite films

Thin films of Ti-Si-N have been prepared by ion beam assisted deposition (IBAD) from two Ti and Si targets. The silicon concentration in the deposited coatings is varied between 0 and 23.7 at.%. The influence of Si content and growth conditions on the microstructure and mechanical properties were investigated using XPS, AFM, XRD and nanoindenter. These nanocomposite coatings exhibit improved mechanical properties in comparison with TiN deposited under the same condition. The hardness measured by nanoindentation reached 42 GPa in Ti-Si-N films containing 11.32 at.% of Si, whereas TiN films only had a value of about 18 GPa. AFM showed that the finest grain size of Ti-Si-N appeared to be 5 nm when Si content was 11.32 at.%. From XPS and XRD results, the microstructures of the high hardness samples were found to consist of nanocrystal TiN grains and amorphous Si₃N₄.     

IBED Si_3N_4和TiN薄膜的成份、结构与摩擦学性能

本文考察了工艺参数对离子束增强沉积（IBED）氮化硅、氮化钛薄膜的成分和微观组织的影响。测定了薄膜的硬度以及薄膜与基体之间结合力，分析了成分和结构与薄膜的硬度和结合力的关系。考察了在不同载荷和速度条件下St_3N_4、TiN薄膜和52100钢试样的摩擦系数和耐磨性。结果显示，与无膜的52100相比，IBEDSt_3N_4和IBEDTiN的耐磨性成倍提高。探讨了薄膜的磨损机理。     

调制周期对TiN/Ti多层膜组织结构和结合力的影响

为了阐明调制周期对薄膜微观组织及薄膜与基体结合力的影响,采用反应磁控溅射在Ti6Al4V基板上交替沉积了Ti层及TiN层制备了TiN/Ti多层膜。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、显微硬度仪和划痕仪测量分析了薄膜的晶体结构、微观组织、硬度以及薄膜与基体之间的结合力。研究结果表明:TiN/Ti多层膜中均存在TiN,Ti和Ti2N 3种相。TiN/Ti多层膜均以柱状晶方式生长,在调制周期较大(5层)时,TiN和Ti层的界面清晰;随着调制周期的减小(层数增加),TiN和Ti层的界面逐渐消失。与单层TiN薄膜相比,多层TiN/Ti薄膜的硬度显著提高;但随着薄膜层数的增加,多层TiN/Ti薄膜硬度略微降低。当调制周期为80nm(30层)时,薄膜与基体的结合力明显提高,达到73N。     

TiAlBN多元膜的性能与组织结构研究

采用电弧离子镀技术、TA5钛合金靶沉积TiAlBN薄膜，研究了这种多元膜的显微硬度、高温氧化性能和组织结构，结果表明：这种多元膜具有优于TiN膜的显微硬度；不同于TiN膜的显微组织，其最显著的特征是存在一些细小的钛滴；双靶工作状态下，这些钛滴与膜之间的融合效果较好，膜层表面孔隙较少；薄膜具有TiN的面心立方结构，与TiN膜相比，具有更加明显的择优取向趋势。     

气相沉积 Ti / TiN 多层薄膜的力学及耐腐蚀性能研究

目的研究多层薄膜的界面对薄膜性能的影响。方法通过直流磁控溅射法在45#钢表面制备Ti N及Ti/Ti N多层薄膜,采用扫描电镜和XRD衍射分析仪对薄膜表面形貌及相结构进行观察和分析,使用纳米压痕仪、电子薄膜应力分布测试仪对Ti N及Ti/Ti多层薄膜的力学性能以及残余应力大小进行研究,并运用电化学设备对Ti N及不同调制周期的Ti/Ti多层薄膜的耐腐蚀性能进行研究。结果制备的Ti N及Ti/Ti N多层薄膜表面光滑且结构致密,Ti N晶粒细小且为非晶相;薄膜力学性能良好,内部均存在残余压应力。随着调制周期的减小,弹性模量和硬度先减小后增大,内部残余应力逐渐减小且分布不均匀程度逐渐增大。薄膜在H_2SO_4中的腐蚀试验表明:当Ti/Ti N多层薄膜调制周期为1μm时,多层薄膜的耐腐蚀性能不如Ti N薄膜,随着Ti/Ti N多层薄膜随调制周期的减小,多层薄膜的耐腐蚀性能逐渐升高;当调制周期为0.5μm时,Ti/Ti N多层薄膜的耐蚀性能已超过Ti N薄膜。结论 Ti/Ti N多层薄膜界面的增多有助于减小薄膜的残余应力,并且可提高薄膜的耐蚀性能。     

直流磁控溅射法在玻璃基片上制备TiN薄膜

采用直流反应磁控溅射法在玻璃片上制备了TiN薄膜,研究不同制备工艺条件与薄膜性能之间的关系。用紫外-可见光分光光度计测试了不同沉积时间和N2流量条件下TiN薄膜透光率;用X射线衍射仪分析了不同N2流量和溅射功率条件下TiN薄膜结构;用扫描电镜(SEM)观察了TiN薄膜的表面腐蚀形貌,用恒电位仪对TiN薄膜的耐腐蚀性进行了分析。结果表明:当沉积时间为2min,N2流量为15mL/min时,在可见光区有较高的透光率,在近红外区的透光率很低;当N2流量为15mL/min,溅射功率为4kW时,TiN薄膜的结晶最致密;当溅射功率为4kW时,TiN薄膜具有较好的耐腐蚀性。     

The Effect of Diffusion Barrier and Bombardment on Adhesive Strength of CuCr Alloy Films

COPPER is a highly promising alternative material toaluminum-based alloys for the new generation of ULSIcircuits owing to its low electrical resistivity and highelectromigration resistance1.However,Cu line or filmcannot completely show its advantages since Cu caneasily diffuse into silicon substrate and the adhesivestrength between Cu and Si is not well enough in somecases.To alloy pure copper with small amounts ofsolutes can not only enhance the electromigrationresistance but also improv…     

低温磁控溅射与普通多弧离子镀TiN薄膜的摩擦学性能比较

采用低温磁控溅射和普通多弧离子镀分别在冷作模具钢基体上制备了TiN薄膜，用纳米压痕法测量了薄膜的表面硬度，并比较了低温磁控溅射与普通多弧离子镀TiN薄膜的摩擦学性能。试验表明，低温磁控溅射TiN薄膜具有与普通多弧离子镀TiN薄膜相近的表面硬度，在多种试验条件下，低温磁控溅射TiN薄膜都有较好的摩擦学性能，摩擦副的磨损率低，摩擦因数小且变化平稳，磨损表面光滑。     

Nanostructured superhard films as typical nanomaterials

The advantages of the use of film samples for nanomaterials science studies are characterized. In particular, nanograined structures are readily obtained in film samples, whereas they are difficult to obtain in bulk samples. The properties of superhard multilayer nitride films, including the deformation of TiN and TiB₂ films during indentation, the effect of an additional external magnetic field on the (TiB₂-B₄C) films' nanostructure and microhardness, as well as galvanomagnetic properties of TiN films are described and discussed in detail. It was found that generally the microhardness of multilayer nitride films increased with the number of layers, except if the two layers mutually dissolved. A microhardness of 78 GPa was achieved in 180 layer TiN/NbN films. TiB₂ films had an inhomogeneous step-like deformation pattern under indentation, in contrast to TiN films, which had a homogeneous deformation pattern, probably due to a slip along columnar grain boundaries. Application of an additional external magnetic field during magnetron sputter deposition increased hardness and smoothness of both crystalline and amorphous (TiB₂-B₄C) films. Decreasing the grain size of TiN films decreased the electron mobility while maintaining the carrier density. The oxygen and carbon distribution can be considered as random in TiN films with the grain size interval of 10-30 nm.     

TaN／TiN和TaWN／TiN多晶超晶格薄膜的微结构与超硬效应

通过磁控反应溅射仪制备了ＴａＮ／ＴｉＮ和ＴＡｗｎ／ＴｉＮ多晶超晶格薄膜。采用Ｘ射线衍射仪。透射电子显微镜和显微硬度仪对超 格薄膜的微结构和硬度进行了分析。     

The dependence of hardness and corrosion protection power of ion- beam-assisted deposition TiN coatings on the ion beam impact angle

Hard coatings such as titanium nitride are often porous and therefore not necessarily very corrosion resistant. Possibilities for reducing the film porosity are densification and multilayer structures. These methods are studied in our laboratories at present.

Ion-beam-assisted deposition (IBAD) TiN films were deposited changing the angle between the substrate normal and the ion beam incidence direction.

The films were characterized by transmission electron microscopy, scanning electron microscopy and X-ray diffraction analyses, the hardness was determined by means of a dynamic Vickers hardness tester and the corrosion behaviour was evaluated using current-potential measurements in a multicycle voltammogram mode.

The results are strongly dependent on the changes in the crystal orientation induced by the ion flux under different angles. Careful optimization may lead to coatings with high hardness and excellent corrosion protection potential. These results are compared with Ti/TiN multilayers deposited by IBAD and magnetron sputtering and with a sputtered TiN single layer.     

金属和陶瓷配副件条件下TiN薄膜的摩擦学特性

多弧离子镀TiN薄膜具有广泛的应用.采用多弧离子镀技术在不锈钢衬底表面沉积了TiN薄膜.用显微硬度计测试了TiN薄膜的硬度,用往复球-盘式摩擦磨损试验机评价了在GCr15和Si3N4两种不同配副件及空气中干摩擦条件下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)和X射线光电子能谱(XPS)观察和测试了磨痕形貌和磨痕处主要化学元素组成,用金相显微镜观察了配副件磨损表面形貌.结果表明:在不同配副件条件下,TiN薄膜的摩擦因数随速度和载荷的增加均出现了降低的趋势.而在相同速度和载荷下,以GCr15为配副件时TiN薄膜的摩擦因数小于以Si3N4为配副件时的摩擦因数.以Si3N4为配副件时TiN薄膜主要表现为磨粒磨损.以GCr15为配副件时TiN薄膜几乎没有磨损,而配副件GCr15主要表现为磨粒与粘着磨损.     

A comparative study of the properties of TiN films deposited by MAIP and FCAP

In this study two types of TiN films were prepared, one using the filtered cathodic arc plasma (FCAP) technique with an in-plane “S” filter, and the other using the multi-arc ion-plating (MAIP), and both deposited under the same parameters. Comparisons of the texture, hardness, roughness, tribological and electrochemical corrosion behaviors of the two types of TiN films were given. The TiN films obtained by the FCAP technology were found to be highly uniform, smooth and macroparticle-free. The TiN films deposited by FCAP had a (111) preferred orientation, while there was no texture in the films deposited by MAIP. Under low load the two kinds of TiN coatings had very different wear mechanisms; the films of FCAP had a lower wear rate and friction coefficient compared with the TiN films deposited by the MAIP technique. The dense and hole-free structure of TiN films of FCAP could effectively avoid the avalanche of TiN films from the substrate during corrosion tests.     

氮化钛薄膜二次电子发射特性研究

目的研究氮化钛薄膜的部分物理特性及真空中的电子发射特性,验证氮化钛薄膜具有相对较好的电导特性及较低的电子发射系数,证明氮化钛薄膜在空间大功率微波器件表面处理中有良好的应用前景。方法使用射频磁控溅射技术在单晶硅及玻璃片表面制备氮化钛薄膜,实验中通过调节溅射过程中氮气与氩气的气体流量比控制薄膜中的氮钛原子比。使用SEM对氮化钛薄膜的表面形貌及厚度进行表征。使用超高真空二次电子发射特性研究平台对氮化钛薄膜的二次电子发射特性进行表征。结果通过调节溅射过程中的氮气氩气流量比,能够有效控制薄膜中氮钛两种元素的含量,进而改变氮化钛薄膜的结晶方式和其他物理特性。当氮氩气体流量比约为10:15时,薄膜中氮钛原子比约为1:1。电阻率测试结果表明,薄膜中氮钛原子比越接近1:1,薄膜的电阻率越低。二次电子产额(SEY)测试结果表明,所制备氮化钛薄膜的最小SEY峰值约为1.46,低于平滑金(~1.8)、银(~2.2)表面的SEY。结论氮化钛薄膜具有较好的电导特性及较低的SEY,且其在真空环境中有良好的稳定性,能在不影响微波器件表面损耗的情况下,有效降低器件表面发生电子倍增的风险。     

ZL109铝合金表面离子镀TiN薄膜及耐磨性

采用多弧等离子体辅助物理气相沉积法,在ZL109铝合金表面沉积了TiN薄膜并对其形貌结构及耐磨性进行了研究。结果表明,在温度较低时TiN薄膜在ZL109铝合金表面生长方式为平面生长模式,随着沉积温度的升高及时间的延长,生长方式向岛状生长模式转化;在沉积温度为280℃,时间为1h时,得到的TiN薄膜厚度在2μm以上;ZL109铝合金表面沉积TiN薄膜后耐磨性提高约4倍。     

ZrN及其多层膜的性质和耐腐蚀性能

用磁过滤电弧制备了ZrN和ZrN／TiN多层膜，磁控溅射制备了ZrN薄膜。结果表明，ZrN／TiN多层膜，由于纳米多层化作用，硬度高于ZrN和TiN的26GPa和2lGPa，平均值达到34．5GPa。X射线衍射分析表明，ZrN／TiN多层膜由ZrN和TiN组成。过滤电弧制备的ZrN和ZrN／TiN多层膜的结合力为8lN和77N，磁控溅射制备的ZrN薄膜的结合力为26N。极化曲线的结果显示，过滤电弧制备的ZrN和ZrN／TiN多层膜的耐腐蚀性显著优于磁控溅射制备的ZrN薄膜，讨论了两种方法制备薄膜性能差异的原因。