Ag/Cu和Cu/Ni纳米金属多层膜强度软化的理论分析

用电沉积法分别制备了具有不同调制波长的Ag/Cu和Cu/Ni金属多层膜,研究了多层膜的硬度与调制波长之间的关系.结果表明,当调制波长λ>300 nm时,两种多层膜的硬度与调制波长符合位错塞积机制的Hall-Fetch关系,当λ<300 nm时,都偏离了Hall-Fetch关系;Ag/Cu和Cu/Ni多层膜分别在λ=50nm和100nm处取得硬度峰值.基于Cheng等人的电子理论分别求出了Ag,Cu和Ni金属晶体的位错稳定的临界晶粒尺寸,进而定量地解释了Ag/Cu和Cu/Ni金属多层膜硬度峰值位置.     

调制波长对Cu／Ni金属多层膜力学性能的影响

用电沉积法在低碳钢基体上制备了具有不同调制波长(一个调制波长等于单层Cu膜与单层Ni膜厚度之和)的Cu/Ni金属多层膜，研究了多层膜硬度与其中单层膜厚度之间的关系。结果表明，当膜厚在亚微米范围内时，Cu/Ni多层膜的屈服强度(为硬度值的1/3)与单层膜厚之间符合基于位错塞积模型的Hall-Pctch(H-P)关系式；而当单层膜厚小于100nm时，屈服强度与膜厚的关系偏离了H-P线性关系。基于程开甲等人位错稳定性理论首次对金属多层膜变形行为偏离Hall-Petch关系的现象作了定量解释。     

双槽电沉积法制备Cu/Ag纳米多层膜

双槽电沉积法制备了不同调制波长的Cu/Ag金属多层膜(Cu膜和Ag膜等厚),用扫描电子显微镜观察了多层膜的层状结构,并研究了不同调制波长下多层膜的显微硬度变化.结果表明:双槽电沉积法制备的Cu/Ag多层膜层状结构明显.当调制波长大于100 nm时,显微硬度随调制波长减小而增加;当小于100 nm时,硬度随调制波长减小而...     

Cu/Ni多层膜中交变应力场对可动位错的制约

Cu／Ni多层膜的强化作用来自于多层膜结构中交变应力场对位错运动的约束．该交变应力场主要包括两部分：在共格界面处由于剪切模量差而导致的镜像力,以及多层膜内由于晶格常数差而形成失配位错网的应力．如果位错在膜层内运动的临界应力值小于交变应力场的约束,位错会被限制在单层膜内运动,多层膜被强化;反之,则位错很容易通过界面到达临近的膜层,多层膜开始出现弱化．交变应力场的变化幅值与多层膜的调制波长相关．理论计算结果表明,Cu／Ni多层膜的临界调制波长为1．9nm,但失配位错网的交变应力场在多层膜的调制波长λ=9nm时振幅达到极值．     

Cu/Ni和Cu/Nb纳米多层膜的应变率敏感性

为研究调制周期和界面结构对纳米多层膜应变率敏感性的影响,采用电子束蒸发镀膜技术在Si基片上制备了不同周期(Λ=4 nm,12 nm,20 nm)的Cu/Ni纳米多层膜,采用磁控溅射技术在Si基片上制备了不同周期(Λ=5 nm,10 nm,20 nm)的Cu/Nb纳米多层膜。在真空条件下,对Cu/Ni纳米多层膜进行了温度分别为200和400℃、时间4 h的退火处理,对Cu/Nb纳米多层膜进行了温度分别为200、400和600℃,时间为4 h的退火处理。采用XRD和TEM表征了Cu/Ni和Cu/Nb纳米多层膜的结构,采用纳米压痕仪获取了不同加载应变率(0.005、0.01、0.05和0.2 s~(-1))下纳米多层膜的硬度。结果表明,应变率敏感性受到界面结构和晶粒尺寸的影响,非共格界面密度提高以及晶粒尺寸变大均可导致应变率敏感性下降。当周期变大时,Cu/Ni纳米多层膜的非共格界面密度提高,晶粒尺寸变大,应变率敏感性指数m减小;当周期变大时,Cu/Nb纳米多层膜的非共格界面密度下降,晶粒尺寸变大,m基本不变。随退火温度上升,Cu/Ni和Cu/Nb纳米多层膜应变率敏感性大体上呈现下降趋势,这是由退火过程中非共格界面密度上升和晶粒长大共同引起的。     

Cu/X(X=Cr,Nb)纳米多层膜力/电学性能的尺度依赖性

利用纳米压痕实验以及四探针法,系统研究了相同层厚Cu/X(X=Cr,Nb)纳米金属多层膜的力学性能(强/硬度)和电学性能(电阻率)的尺度依赖性.微观分析表明:Cu/X多层膜调制结构清晰,Cu层沿{111}面择优生长,X层沿{110}面择优生长.纳米压入结果表明,Cu/X多层膜的强度依赖于调制周期,并随调制周期的减小而增加.多层膜变形机制在临界调制周期(λ~c≈25 nm)由Cu层内单根位错滑移转变为位错切割界面.多层膜的电阻率不仅与表面/界面以及晶界散射相关,而且在小尺度下受界面条件显著影响.通过修正的FS-MS模型可以量化界面效应对多层膜电阻率的影响.Cu/X纳米多层膜可以通过调控微观结构实现强度-电导率的合理匹配.     

溅射沉积Cu/W纳米多层膜结构与性能

以单晶硅和聚酰亚胺为衬底,用磁控溅射沉积调制周期λ=25~150 nm、调制比η=0.5~2的Cu/W纳米多层膜,用XRD、SEM、EDS、AFM、微力测试系统、纳米压痕仪和四探针法对多层膜微观结构、表面形貌和力学及电学性能进行研究。结果表明:λ和η显著影响多层膜结构和性能。多层膜Cu层和W层均为纳米晶结构,分别呈Cu(111)和W(110)择优取向。W(110)晶面间距减小且减幅与1/λ或η值呈正相关,Cu/W层间界面处存在扩散混合层。表面Cu层晶粒尺寸随Cu层厚增加而增大。裂纹萌生临界应变εc总体上随λ增大或η减小而下降,屈服强度σ0.2、显微硬度H和电阻率ρ总体上均与λ或η呈负相关。因Cu层和W层厚度随λ或η的变化而改变,相应地改变了Cu层晶粒度及其晶界密度、W层体积分数和Cu/W层间界面数量,使位错运动能力及电子散射效应变化,最终改变Cu/W纳米多层膜性能。     

NbMoWTa/Ag自润滑纳米多层膜的力学性能及摩擦学行为∗

为提高高熵合金薄膜 NbMoWTa 的耐磨减摩性能,采用磁控溅射技术在 Si 基体上制备具有不同调制波长的 NbMoWTa / Ag 纳米多层膜,利用 XRD、SEM 和 TEM 等对纳米多层膜进行表征,分析其硬度和摩擦学性能。 结果表明不同调制周期结构的纳米多层膜结晶性良好。 多层膜硬度随着单层膜厚度 (100~ 5 nm)的降低而增加(5. 62 ~ 8. 39 GPa),在单层膜厚度减小到 20 nm 时,其塑性变形机制由位错在界面处的堆积机制转变为位错穿越界面运动机制;在尺寸小于 10 nm 时,多层膜的硬度接近于高熵合金 NbMoWTa 单质膜 (10. 93 GPa),这可能由随着单层厚度的降低引起 NbMoWTa 膜与 Ag 膜之间界面由半共格向共格转变所引起。 同时,通过摩擦磨损试验获得纯 NbMoWTa 薄膜的摩擦因数为 0. 49,磨损率为 1. 75×10^-5 mm³N^-1m^-1 ;单层膜厚度为 5 nm 的多层膜的摩擦因数为 0. 23,磨损率为 2. 19×10^-5 mm³N^-1m^-1 。 在 NbMoWTa 中添加 50%的 Ag 制备而成的纳米多层膜有共格强化效应,保证了其高硬度高强度的同时,由多层设计实现了耐磨和自润滑的协同控制。     

不同退火温度下Cu/Ni纳米多层膜的结构与力学性能稳定性

为研究不同退火温度下Cu/Ni纳米多层膜的结构与力学性能稳定性,采用电子束蒸发镀膜技术在Si(100)基片上沉积不同周期(Λ为4,12,20 nm)的Cu/Ni多层膜,在真空条件下对试样进行温度为200℃和400℃,时间为4 h的退火处理,分析了沉积态(未退火态)与退火态Cu/Ni多层膜纳米压痕硬度、弹性模量与微结构的演变,讨论了不同调制周期Cu/Ni多层膜的热稳定性。结果表明:200℃下4 h退火后,Λ为4,12和20 nm的Cu/Ni多层膜均保持了硬度与弹性模量的热稳定性。而在400℃下4 h退火后,Λ为12 nm的Cu/Ni多层膜出现了硬度和弹性模量的软化现象,硬度由6.21 GPa降低至5.83 GPa,弹性模量由190 GPa降低至182 GPa。这是由于共格界面被破坏,界面共格应力对Cu/Ni多层膜力学性能贡献作用削弱导致的。     

Cu/Ni多层膜对Ti811合金微动磨损和微动疲劳抗力的影响

在Ti811钛合金表面利用离子辅助磁控溅射沉积技术制备20～1200nm不同调制周期的Cu/Ni金属多层膜,分析多层膜的结构,测试膜基结合强度、膜层显微硬度和韧性,对比研究不同调制周期的Cu/Ni多层膜对钛合金基材常温下微动磨损性能和微动疲劳(FF)抗力的影响。结果表明:利用离子辅助磁控溅射技术可以获得致密度高、晶粒细化、膜基结合强度高的Cu/Ni多层膜,该类多层膜具有良好的减摩润滑作用,因而改善了Ti811钛合金常温下抗微动磨损和微动疲劳性能;Cu/Ni多层膜对钛合金FF抗力的改善程度随膜层调制周期呈现非单调变化趋势,调制周期为200nm的Cu/Ni多层膜对钛合金FF抗力的提高程度最大,原因归于该膜层具有良好的强韧和润滑综合性能。     

Electron theory based explanation and experimental study on deformation behavior of Cu/Ni multilayers

Cu/Ni multilayers with various defined thickness of Cu and Ni layers were electrodeposited on low carbon steel substrates. Hardness measurements indicated that the increase in yield strength (one-third of hardness) with a decrease of layer thickness for Cu/Ni multilayers with single layer thickness at sub-micron length scale could be described by the Hall-Petch formula of the dislocation pile-up model. In the regime of few tens to a hundred nanometers of single layer thickness, the dislocation pileup-based Hall-Petch model broke down. This could be explained quantitatively according to the criterion condition on the limit size of dislocation derived from a modified Thomas-Fermi-Dirac electron theory.     

Interfacial Structures Governed Plastic Deformation Behaviors in Metallic Multilayers

In this work, we have investigated the mechanical properties of Cu/Ta, Ag/Cu and Ag/Nb multilayers with different heterogeneous interfaces. The results suggest that when individual layer thickness(h) is larger than 5–10 nm, the hardness/strength of three different multilayer systems has the similar length scale effect with decreasing layer thickness,while when h B 5 nm, the three multilayer systems show remarkably different plastic deformation behaviors. The strength curves exhibit the variation trends of unchanging, softening and increasing corresponding to Cu/Ta, Ag/Cu and Ag/Nb multilayers, respectively. The microstructure analysis shows that three kinds of multilayers have totally different interfacial structures, which lead to the different strengthening or softening mechanisms.     

Tensile testing of free-standing Cu,Ag and Al thin films and Ag/Cu multilayers

Free standing polycrystalline thin films with a strong 〈111〉 texture were tested in uniaxial tension. Studied were electron-beam deposited Ag, Cu and Al films, and Ag/Cu multilayers consisting of alternating Ag and Cu layers of equal thickness, between 1.5 nm and 1.5 μm (bilayer repeat length, λ, between 3 nm and 3 μm). The films had a total thickness of about 3 μm. A thin polymeric two-dimensional diffraction grid was deposited on the film surface by microlithographic techniques. Strains were measured in situ from the relative displacements of two laser spots diffracted from the grid. The average values of the Young’s moduli, determined from hundreds of measurements, are 63 GPa for Ag, 102 GPa for Cu, 57 GPa for Al and 87.5 GPa for Ag/Cu multilayers. In all cases, these values are about 20% lower than those calculated from the literature data and, for the Ag/Cu multilayers, are independent of λ. No “supermodulus” effect was observed. The 20% reduction in modulus is most likely the result of incomplete cohesion (“microcracking”) of the grain boundaries. The ductility of the Ag/Cu multilayers decreases when λ is reduced. For λ<80 nm, the films are brittle at room temperature: they break without macroscopic plastic flow. For λ>80 nm, the yield stress increases with decreasing λ according to a Hall–Petch-type relation. No softening with decreasing grain size was observed even at the lowest values of λ.     

Microstructures and strength of nanoscale Cu–Ag multilayers

Cu–Ag multilayers were found to have lower peak hardness than Cu–Ni in spite of lower misfit dislocation spacing that is expected to increase the resistance of interfaces to glide dislocation transmission. This is attributed to misfit dislocation core spreading in the interface plane in Cu–Ag.     

Magnetron sputtering deposition of [FePt/Ag]n multilayers for perpendicular recording

[FePt/Ag]n multilayers were deposited on glass substrates by RF magnetron sputtering and ex situ annealed at 550℃ for 30 min. The effects of inserted Ag layer thickness and the number of bilayer repetitions （n） on the structure and magnetic properties of the multilayers were investigated. It was found that the difference between in-plane and out-of-plane coercivities varied with an increase of inserted Ag layer thickness in the [FePt 2 nm/Ag x nm]10 multilayers. The ratio of out-of-plane coercivity to in-plane coercivity reached the maximum value with the Ag layer thickness of 5 nm, indicating that the Ag layer thickness plays an important role in obtaining perpendicular orientation. For the [FePt 2 nm/Ag 5 um]n multilayers, perpendicular orientation is also influenced by n. The maximum value of the ratio of out-of-plane coercivity to in-plane coercivity appeared when n was given as 8. It was found that the [FePt 2 nm/Ag 5 nm]8 had a high perpendicular coercivity of 520 kA/m and a low in-plane one of 88 kA/m, which shows a strong perpendicular anisotropy.     

Analytic treatment of metallic multilayer strength at all length scales: Influence of dislocation sources

Metallic multilayers exhibit a very pronounced size effect where the mechanical strength depends on the layer thickness. Traditionally the Hall–Petch relation is used to account for the size effect. However, rigorous application of dislocation pileup theory predicts significant deviation from the Hall–Petch relation due to elastic inhomogeneity, discreteness of dislocations and dislocation source operation. Elastic inhomogeneity leads to anomalous scaling where the scaling exponent deviates from 1/2 of the classical Hall–Petch relation. The discrete dislocation effect is properly accounted for by a piecewise approach that can be applied at all length scales. In this article, a key step in the formulation is taken: the dislocation source characteristics are taken into consideration. Thus, all the three effects are accounted for. Analytic formulas linking yield stress to microscopic interface strength, dislocation source activation stress and other easily obtainable parameters (the Burgers vector, the elastic constants of constituent materials, crystal structure and layer thickness) are provided for all length scales. The model is then applied to Cu/Ni multilayers and the predicted strength is compared with experimental data.     

Cu/Nb纳米金属多层膜延性及断裂行为的尺寸效应

通过单轴拉伸实验并结合原位电阻测量法系统研究了恒定调制比下调制波长(λ=10-250 nm)对聚酰亚胺基体上Cu/Nb纳米金属多层膜延性和断裂韧性的影响.微观分析表明,Cu/Nb的调制结构清晰,不存在明显的互混现象.实验结果表明,随着调制波长的减小,多层膜的延性和断裂韧性均呈现非单调演变趋势,在调制波长为50 nm左右...     

退火时间对块体纳米晶Fe3Al材料组织性能的影响

在800℃下对铝热反应法制备的含10%Ni的纳米晶Fe3Al材料进行了不同时间的等温热处理,保温时间分别为4、8、12、16、20、24和48 h。利用XRD和TEM分析了不同保温时间下材料的平均晶粒尺寸,并对硬度进行了测试,研究了晶粒尺寸变化趋势以及硬度变化规律,探讨了两者之间的变化关系。结果表明:材料的平均晶粒尺寸在不同时间的退火处理后,呈现出两次减小,两次增大,最后趋于平稳的过程。晶粒尺寸在4 h等温处理后达到最小值16 nm,在24 h等温处理后达到最大值35 nm。存在一个临界值dc=20 nm,当晶粒尺寸小于dc时,维式硬度和晶粒尺寸之间满足反Hall-Petch关系,当晶粒尺寸大于dc时,两者之间呈现正的Hall-Petch关系。16 h退火处理后维氏硬度最大为490 HV,24 h退火后维氏硬度最小为410 HV。