W/SiC纳米多层膜的制备及表征

采用多靶磁控溅射制备了 Ｗ／ＳｉＣ纳米多层膜。并用 ＸＲＤ和 ＴＥＭ研究了 Ｗ／ＳｉＣ纳米多层膜的微结构。研究表明,Ｗ／ＳｉＣ纳米多层膜的调制结构界面平直、清晰、周期性好;ＳｉＣ调制层为非晶态,Ｗ调制层在大调制周期为纳米晶,并随调制周期减小逐渐转变为非晶态。     

W／SiC纳米多层膜的制备及表征

采用多靶磁控溅射制备了Ｗ／ＳｉＣ纳米多层膜,并用ＸＲＤ和ＴＥＭ研究了Ｗ／ＳｉＣ纳米多层膜的微结构。研究表明,Ｗ／ＳｉＣ纳米多层膜的调制结构界面平直,清晰,周期性好,ＳｉＣ调制层为非晶态,Ｗ调制层在大调制周期为纳米晶,并随调制周期减小逐渐转变为非晶态。     

Ti—Mo—N三元多层膜的结构与性能

采用Ｔｉ／Ｍｏ复合靶,用多弧离子镀技术沉积了Ｔｉ－Ｍｏ－Ｎ多元多层膜,并对其组织结构与性能进行了研究,结果表明：在本试验条件下多元膜的结构形式为（Ｔｉ,Ｍｏ）２Ｎ,最佳多层膜的结构形式为基体／Ｔｉ／ＴｉＮ／（ＴｉｙＭｏ１－７）Ｎ／（Ｔｉ,Ｍｏ）２Ｎ,并具有较高的显微硬度、耐磨性和极低的孔隙率,在８００℃具有很好的抗氧化性能。在沉积过程中存在着多元合金膜层与合靶的成分离析现象,这与靶材的结构有关。     

TiN/NbN纳米多层薄膜的交变应力场和超硬效应

为了研究纳米多层薄膜的超硬效应 ,采用反应溅射法制备从 1 4nm至 2 7nm不同调制周期的一系列TiN/NbN纳米多层膜。高分辨电子显微镜对薄膜的调制结构和界面生长方式的观察发现 ,TiN/NbN膜具有很好的调制结构 ,并呈现以面心立方晶体结构穿过调制界面外延生长的多晶超晶格结构特征。显微硬度测量表明 ,TiN/NbN纳米多层膜存在随调制周期变化的超硬效应。薄膜在调制周期为 8 3nm时达到HK39 0GPa的最高硬度。分析认为 ,两种不同晶格常数的晶体外延生长形成的交变应力场 ,对材料有强化作用 ,这是TiN/NbN纳米多层膜产生超硬效应的主要原因     

SiO2层晶化对TiN/SiO2纳米多层膜结构和性能的影响

采用多靶磁控溅射法制备了一系列具有不同SiO2调制层厚的TiN/SiO2纳米多层膜.利用X射线衍射、X射线能量色散谱、扫描电子显微镜、高分辨电子显微镜和微力学探针表征和研究了多层膜的生长结构和力学性能.结果表明,具有适当厚度(0.45～0.9 nm)的SiO2调制层,在溅射条件下通常为非晶态,在TiN层的模板作用下晶化并与TiN层共格外延生长,形成具有强烈(111)织构的超晶格柱状晶多层膜;与此相应,纳米多层膜产生了硬度和弹性模量异常增高的超硬效应(最高硬度达45 GPa).随着SiO2层厚度的继续增加,SiO2层转变为非晶态,阻断了多层膜的共格外延生长,使纳米多层膜形成非晶SiO2层和纳米晶TiN层的多层结构,多层膜的硬度和弹性模量逐渐下降.     

NiFe／Cu和NiFe／Mo多层膜的界面结构与巨磁电阻

采用磁控溅射方法制备了ＮｉＦｅ／Ｃｕ和ＮｉＦｅ／Ｍｏ多层膜。测量了厚度不同的Ｃｕ层和Ｍｏ层多层膜的磁性和磁电阻,并用电镜分析了部分ＮｉＦｅ／Ｃｕ多层膜样品。测量到ＮｉＦｅ／Ｃｕ多层膜的室温巨磁电阻随Ｃｉ层厚度振荡的第一、二、三峰。而在ＮｉＦｅ／Ｍｏ多层膜中未发现巨磁电阻效应。讨论了多层膜的界面结构对巨磁电阻效应的影响。     

TiN／NbN纳米多层薄膜的交变应力场和超硬效应

为了研究纳米多层薄膜的超硬效应，采用反应溅射法制备从1.4nm至27nm不同调制周期的一系列TiN/NbN纳米多层膜。高分辨电子显微镜参薄膜的调制结构和界面生长方式的观察发现，TiN/NbN膜具有很好的调制结构，并呈现以面心立方晶体结构穿过调制界面外延生长的多晶超晶格结构特征。显微硬度测量表明，TiN/NbN纳米多层膜存在随调制周期变化的超硬效应。薄膜在调制周期为8.3nm时达到HK39.0 Gpa的最高硬度。分析认为，两种不同晶格常数的晶体外延生长形成的交变应力场，对材料有强化作用，这是TiN/NbN纳米多层膜产生超硬效应的主要原因。     

c-AIN的生长对AIN/(Ti,Al)N纳米多层膜力学性能的影响

采用反应磁控溅射制备了具有不同调制周期的AIN/(Ti,Al)N纳米多层膜,研究了亚稳相立方氮化铝(c-AIN)在纳米多层膜中的生长条件及其对薄膜力学性能的影响。结果表明:在小调制周期下AIN以立方结构存在,并与(Ti,Al)N层形成同结构共格外延生长,使纳米多层膜产生较大的晶格畸变。与此相应,AIN/(Ti,Al)N纳米多层膜硬度和弹性模量随调制周期的减小呈单凋上升的趋势,当调制周期小于8～10 nm时其增速明显增大,并在调制周期为1.3 nm时达到最高硬度29.0GPa和最高弹性模量383 GPa.AIN/(Ti,Al)N纳米多层膜的硬度和弹性模量在小调制周期时的升高与亚稳相c-AIN的产生并和(Ti,Al)N形成共格结构有关。     

离子束溅射制备Co／Pt多层膜的结构和磁性

采用离子束溅射技术制备了Ｃｏ／Ｐｔ多层膜，并研究了多层膜的结构和磁性随Ｃｏ层厚度或Ｐｔ层厚度的变化关系。结果表明Ｃｏ层呈现出ｈｃｐ结构的（００２）结构，Ｐｔ层表现出ｆｃｃ结构的（１１１）织构。当Ｃｏ层和Ｐｔ层都比较薄时，界面有Ｃｏ－Ｐｔ的化合物形成。     

陶瓷硬质纳米多层膜研究进展

陶瓷纳米多层膜因具超硬效应而成为近年的研究热点.本文对这类人工材料的研究进展和存在的不足进行了评述,并展望了进一步研究的方向.二十年来,陶瓷纳米多层膜的实验研究已取得明显进展:在微结构特征方面,两调制层形成共格外延生长结构是纳米多层膜产生超硬效应的必要微结构条件已成为共识;材料组合方面,由于模板效应,不同结构类型的材料,甚至非晶材料都可在纳米多层膜中形成共格外延生长结构,高硬度纳米多层膜材料体系已得到大大的拓展.与此相比较,对纳米多层膜强化机制和设计准则的研究相对滞后,仍停留在以金属纳米多层膜基于位错运动受阻于界面的理论解释上.因而,建立适合于陶瓷纳米多层膜的强化机制和设计准则;拓展纳米多层膜的材料组合,开发以碳化物、硼化物甚至氧化物为基的纳米多层膜将成为进一步研究的方向.     

Investigation of Mo/Si and W/Si interfaces by phase modulated spectroscopic ellipsometry and cross-sectional transmission electron microscopy

Mo and W thin films and Mo/Si/Mo and W/Si/W tri-layers have been deposited by r.f. magnetron sputtering on c-Si substrates as a precursor to the fabrication of Mo/Si and W/Si multilayer X-ray mirrors. The Phase Modulated Spectroscopic Ellipsometry (SE) technique has been used for characterizing the single layer films to derive information regarding the thickness and volume fraction of voids present in the surface layers. The Mo/Si/Mo and W/Si/W tri-layer structures have been characterized by the Cross-sectional Transmission Electron Microscopy (XTEM) technique. The inter-diffusion at the interfaces of the tri-layer structures observed by the XTEM technique has been correlated to the thickness of the surface layers of the metal films obtained from the SE measurement.     

基于Al／MoOx纳米复合薄膜的含能半导体桥研究

使用微细加工和磁控溅射技术将Al/MoO x纳米复合薄膜集成于半导体桥(SCB),制成含能半导体桥SCB-Al/MoO x以提高SCB的点火能力。薄膜的SEM、DCS和XPS结果表明,复合薄膜成膜质量好,层状结构清晰,放热量可达3200 J/g,达到理论值的68%(理论放热量为4703 J/g),MoO x薄膜含有32%的MoO3、37%的Mo2O5以及31%的MoO2。电容激励发火实验表明:相同激发条件下,SCB-Al/MoO x反应终止时间较SCB显著缩短,能量输出效率高于SCB,发火时溅射出的火花量明显增多,持续时间显著延长,使用原子发射双谱线测温法得到的等离子体温度亦高于SCB。     

具有纳米调制结构的AlTiN/AlCrN复合涂层在干摩擦条件下的摩擦磨损性能研究

目的 研究干摩擦条件下不同AlTiN/AlCrN多层膜纳米调制结构对摩擦磨损行为的影响。方法 将处理过的合金工具钢和单晶硅片作为膜层生长的基底材料,在膜层制备之前,先对基底材料进行预处理,然后使用多靶磁控溅射纳米膜层系统沉积一系列不同调制周期和调制比的AlTiN/AlCrN纳米多层膜。通过控制涂层总厚度不变,在调制比为1︰1时,设计不同的调制周期,择优选出磨损量最小、耐磨性最好的调制周期,并以此为恒定值,进而设计不同调制比的试样。采用X射线衍射仪(XRD)、摩擦磨损试验机分析与表征纳米多层膜的微观结构和性能,研究调制周期和调制比对AlTiN/AlCrN纳米多层膜微观结构和干摩擦条件下摩擦磨损性能的影响。结果 AlTiN/AlCrN纳米多层膜主体均为面心立方结构,且在(111)、(200)和(220)晶面择优取向。调制结构对多层膜的磨损特性影响较大,当调制周期为14.4 nm时,在干摩擦条件下AlTiN/AlCrN纳米多层膜的摩擦磨损量最小;在调制周期恒定为14.4 nm情况下,当调制比为3︰1时,在干摩擦条件下AlTiN/AlCrN纳米多层膜的耐磨性能最好;AlTiN/AlCrN纳米多层膜的磨损机理主要以磨粒磨损和黏附磨损为主。结论 优化的AlTiN/AlCrN多层膜纳米调制结构技术可应用在切削刀具的表面再制造领域,从而延长刀具工作寿命,通过涂层良好的耐磨性能提升设备的加工效率。     

Crystallization of chemically vapor deposited molybdenum and mixed tungsten/molybdenum oxide films for electrochromic application

The paper deals with investigation of Mo oxide and mixed W/Mo oxide films showing high electrochromic performance. Films are deposited on Si and conductive glass substrates using pyrolytical decomposition at 200 °C of Mo and W hexacarbonyls in Ar/O₂ atmosphere. The study is focused on structural transformation of the films in dependence on deposition and annealing process parameters. In case of conductive glass substrate (typical for electrochromic devices), the crystallization process in Mo oxide films is almost completed at 400 °C forming triclinic MoO_2.89 and orthorhombic MoO₃ crystalline phases. The structure of mixed W/Mo oxide films is triclinic crystalline phase of tungsten oxide matrix with Mo atoms as substitutes. Discussed are, as well, differences in the crystallization process for the same films, when the substrate is Si. All the films show electrochromic effect, the mixed W/Mo oxide films expressing stronger electrochromic effect with superior color efficiency and optical modulation.     

掺杂氧化钨薄膜的电致变色特性

掺杂氧化钼对氧化钨薄膜的电致变色特性有一定的影响,本文介绍了用电子束蒸发制备不同MoO3掺杂比例的氧化钨膜,对其着色态与漂白态的光学特性以及循环伏安特性进行了实验研究,通过对循环伏安曲线的分析,对杂氧化钨薄膜电致变色的机理进行了讨论。     

Recovery of Multilayer-Coated Zerodur and ULE Optics for Extreme-Ultraviolet Lithography by Recoating, Reactive-Ion Etching, and Wet-Chemical Processes

Extreme-ultraviolet lithography requires expensive multilayer-coated Zerodur or ULE optics with extremely tight figure and finish specifications. Therefore it is desirable to develop methods to recover these optics if they are coated with a nonoptimum multilayer films or in the event that the coating deteriorates over time owing to long-term exposure to radiation, corrosion, or surface contamination. We evaluate recoating, reactive-ion etching, and wet-chemical techniques for the recovery of Mo/Si and Mo/Be multilayer films upon Zerodur and ULE test optics. The recoating technique was successfully employed in the recovery of Mo/Si-coated optics but has the drawback of limited applicability. A chlorine-based reactive-ion etch process was successfully used to recover Mo/Si-coated optics, and a particularly large process window was observed when ULE optics were employed; this is an advantageous for large, curved optics. Dilute HCl wet-chemical techniques were developed and successfully demonstrated for the recovery of Mo/Be-coated optics as well as for Mo/Si-coated optics when Mo/Be release layers were employed; however, there are questions about the extendability of the HCl process to large optics and multiple coat and strip cycles. The technique of using carbon barrier layers to protect the optic during removal of Mo/Si in HF:HNO(3) also showed promise.     

C/C复合材料高温长寿命抗氧化复合涂层研究

采用包埋技术在C/C复合材料表面制备SiC-WSi₂/MoSi₂抗氧化复合涂层; 通过恒温氧化实验以及X射线衍射分析、扫描电镜观察及能谱分析, 研究了W、Mo含量对复合涂层微观结构和高温抗氧化性能的影响. 结果表明: 随着包埋粉料中W、Mo含量的增加, 所制备复合涂层的厚度先增加后减小; 含有10.0at％ W和Mo制备的复合涂层具有相对较大的厚度和较为致密的结构, 且WSi₂和MoSi₂含量相对较高; 氧化过程中在涂层表面形成致密和稳定的SiO₂玻璃保护膜; 在1500℃氧化315h后, 带有该涂层的C/C试样仍然没有失重, 且经过18次1500℃←→室温急冷急热后涂层没有开裂和脱落, 说明该涂层具有优异的抗氧化和抗热震性能.     

Effect of tungsten on the electrochromic behaviour of sol-gel dip coated molybdenum oxide thin films

The paper describes the results obtained on the performance of Mo oxide and mixed W/Mo oxide thin films for possible electrochromic applications. Mo and W/Mo oxide films were deposited on conductive (FTO) glass substrates using sol-gel dip coating method. The films were annealed at 250 °C for 30 min. The structure and morphology of Mo and W/Mo oxide films were examined using XRD, SEM and EDS. XRD results indicate the amorphous nature of the Mo and W/Mo oxide films annealed for 30 min. The CV measurements revealed that the films prepared with 10 wt.% of tungsten exhibit maximum anodic/cathodic diffusion coefficient of 24.99/12.71 × 10⁻¹¹ cm²/s. The same film exhibits a maximum transmittance variation (ΔT%) of 83.4% at 630 nm and 81.06% at 550 nm with the optical density of 1.00 and 1.13 respectively.     

Mo/Si and Mo/Be multilayer thin films on Zerodur substrates for extreme-ultraviolet lithography

Multilayer-coated Zerodur optics are expected to play a pivotal role in an extreme-ultraviolet (EUV) lithography tool. Zerodur is a multiphase, multicomponent material that is a much more complicated substrate than commonly used single-crystal Si or fused-silica substrates. We investigate the effect of Zerodur substrates on the performance of high-EUV reflectance Mo/Si and Mo/Be multilayer thin films. For Mo/Si the EUV reflectance had a nearly linear dependence on substrate roughness for roughness values of 0.06-0.36 nm rms, and the FWHM of the reflectance curves (spectral bandwidth) was essentially constant over this range. For Mo/Be the EUV reflectance was observed to decrease more steeply than Mo/Si for roughness values greater than approximately 0.2-0.3 nm. Little difference was observed in the EUV reflectivity of multilayer thin films deposited on different substrates as long as the substrate roughness values were similar.     

Survey of Ti-, B-, and Y-based soft x-ray-extreme ultraviolet multilayer mirrors for the 2- to 12-nm wavelength region

We have performed an experimental investigation of Ti-, B(4)C-, B-, and Y-based multilayer mirrors for the soft x-ray?extreme ultraviolet (XUV) wavelength region between 2.0 and 12.0 nm. Eleven different material pairs were studied: Ti/Ni, Ti/Co, Ti/Cu, Ti/W, B(4)C/Pd, B/Mo, Y/Pd, Y/Ag, Y/Mo, Y/Nb, and Y/C. The multilayers were sputter deposited and were characterized with a number of techniques, including low-angle x-ray diffraction and normal incidence XUV reflectometry. Among the Ti-based multilayers the best results were obtained with Ti/W, with peak reflectances up to 5.2% at 2.79 nm at 61° from normal incidence. The B(4)C/Pd and B/Mo multilayer mirrors had near-normal incidence (5°) peak reflectances of 11.5% at 8.46 nm and 9.4% at 6.67 nm, respectively, whereas a Y/Mo multilayer mirror had a maximum peak reflectance of 25.6% at 11.30 nm at the same angle. The factors limiting the peak reflectance of these different multilayer mirrors are discussed.