金属多层膜力学行为及其组元与尺寸效应
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摘要
金属薄膜材料由于其优异的力/电学性能，已成为目前高性能微元器件、微机电系统以及互连结构的核心材料体系，其在复杂的微加工制备和随后的服役过程中的变形损伤，是导致系统失效的关键因素。作为其组成单元，多层膜及其组元材料介观服役特性研究具有重要的科学意义和工程实用价值。本论文选取微电子器件中典型应用的Cu薄膜及Cu/X (X=Cr、Nb、Zr)多层膜材料为研究对象，系统研究了其介观尺度下的力/电学行为及相关的物理机理。
通过单轴拉伸和机械疲劳实验系统研究了介观尺度Cu薄膜的力学性能。结果表明，Cu薄膜的屈服强度以及疲劳行为（疲劳寿命与疲劳损伤）均表现出明显的尺寸依赖性。屈服强度以及疲劳寿命在某一临界尺寸下出现最大值。室温以及低应变速率下，纳米晶Cu薄膜呈现出变形孪晶的双反（晶粒）尺寸效应。根据经典的位错理论以及受激滑移模型，半定量解释了面心立方金属变形孪晶的双反（晶粒）尺寸效应。随着特征尺寸的减小，由于位错活动受到抑制以及可激活位错源的减少，疲劳损伤由位错滑移导致的挤出/侵入转变为与界面相关的损伤。
在单轴拉伸实验过程中利用薄膜电阻实时测量法，初步探索了不同体系Cu/X纳米多层膜的变形与断裂行为及其尺寸效应。研究发现，Cu/X纳米多层膜的屈服强度强烈依赖于其特征结构参数（调制周期与调制比），随调制周期的减小或者调制比的增加（即硬相体积分数增加）而增加，并伴随着变形机制的变化。这与通过约束层滑移模型和复合材料混合强度法则理论计算的结果相一致。由于软/延性相(Cu)对硬/脆性相(X)的异质约束作用，导致Cu/X纳米多层膜的延性以及断裂韧性随特征尺寸变化表现出奇异性，并且出现由张开型向剪切型断裂的转变。通过微观断裂力学模型定量阐述了软/延性相对硬/脆性相的约束作用对断裂行为的影响。此外，调制周期恒定的Cu/X纳米多层膜的强度与延性存在线性关系。界面约束越强（界面数量越多），线性关系的斜率越大。
纳米压痕实验揭示了界面结构对Cu/X (X=Cr、Nb)纳米多层膜的硬度及压入模量的影响。结果表明，Cu/X纳米多层膜的硬度呈现尺寸依赖性并随特征尺寸的减小达到饱和值，其变化趋势与屈服强度相同。与界面清晰的Cu/X多层膜单调变化的压入模量不同，界面混合（非晶）层导致Cu/X多层膜的压入模量出现最大值。通过考虑界面混合（非晶）层引起的组元层晶面间距压缩以及自由体积这两个竞争机制的相互作用，定性解释了压入模量的这种异常变化。
采用金属薄膜原位电阻变化法，通过机械疲劳试验研究了Cu薄膜和Cu/X (X=Cr、Nb)纳米多层膜的疲劳性能。结果表明，与块体材料相似，Cu/X纳米多层膜的疲劳寿命与应变幅仍然遵循经典的Coffin-Mason疲劳关系式，这与Cu薄膜是一致的。合理的强度和延性匹配能够实现薄膜材料疲劳性能的最优化。由于层间异质界面对位错活动的强烈抑制，Cu/X纳米多层膜的疲劳损伤由晶界/界面主导。
利用电阻四探针法系统研究了Cu/X (X=Cr、Nb)纳米多层膜的电输运行为及其尺寸效应。理论分析和实验结果均表明Cu/X纳米多层膜的电阻率均随着调制周期的减小而增加。界面结构可以显著影响纳米多层膜的电阻率。通过人工调控纳米多层膜的微观结构可以实现其力-电综合性能的最优化。
The single-/multi-layered films are widely used as essential components of high performancemicroelectronics, microelectromechanical systems and interconnect structures owing to theiroutstanding mechanical/electric properties. The deformation and fracture during themanufacture and service processes has been identified as an important factor influencingtheir reliability. The urgent demand for understanding the complex properties of thenanostructured multilayers and their constituent are both for scientific aspects and in theinterest of the engineering application. In this work, the mesoscaled mechanical/electronicproperties and the related physical mechanisms of nanocrystalline Cu films andnanostructured Cu/X (X=Cr, Nb, Zr) multilayers that typically used in microelectronicshave been investigated.
Uniaxial tensile test and mechanical fatigue test was respectively performed on themesoscaled Cu thin films to systemically investigate their mechanical properties. It isrevealed from the results that the yield strength of Cu thin films as well as the fatiguebehavior (fatigue lifetime and fatigue damage) is length scale-dependent. Maxima areobserved for both the yield strength and fatigue lifetime in mesoscaled Cu thin films at somecritical dimension. At room temperature and low strain rates, the nanocrystalline Cu thinfilms exhibit the double-inverse deformation twinning behavior with respect to the normalHall-Petch grain size dependence, which is semiquantitatively explained by the classicdislocation theory and dislocation stimulated slip model.With reducing the characteristicdimensions of Cu thin films, the fatigue damage of mesoscaled Cu thin films show thetransition from dislocation glide-induced extrusions/intrusions to boundary related damagedue to the inhibition of dislocation mobility and the limited availability and activation ofdislocation sources.
Uniaxial tensile test with combination of in-situ measurement the change of electricalresistance method was carried out to investigate the deformation and fracture behavior ofnanostructured Cu/X (X=Cr, Nb, Zr) multilayers. It is found that the yield strength of Cu/Xmultilayers strongly depends on the characteristic parameters (modulation period, λ andmodulation ratio, η), i.e., it increases with decreasing the modulation period or increasing themodulation ratio (or increasing the volume fraction of hard phase), accompanied with thetransition of deformation mechanism. This consists with the prediction by the confined layer slip model and the rule of mixture. Due to the constraint effects of soft/ductile phase (Cu) onhard/brittle phase (X), the nanostructured Cu/X multilayers present singularity ductility aswell as fracture toughness, and also show the transition of fracture mode from shearing toopening related to the length scale. The fracture behavior in Cu/X multilayers isquantitatively assessed using a fracture mechanism-based micromechanical model. Moreover,at a constant modulation period, Cu/X multilayers exhibit ductility scaling linearly with yieldstrength that is varied with modulation ratio. The scaling slope for Cu/X multilayers withmore interfaces is much sharper than that of ones with fewer interfaces, owing to a strongerinterface constraint caused by more interfaces.
The nanoindentation test was adopted to explore the effect of interface structure ofnanostructured Cu/X (X=Cr, Nb) multilayers on hardness and modulus. It is revealed thatthe hardness is also length scale-dependent, similar to that of yield strength. Different fromthe monotonic modulation period dependence known for Cu/X multilayers with clearinterface, a maximum indentation modulus is found in the Cu/X multilayers with theinterfacial intermixing (amorphous) layer. This unusual behavior is explained by consideringthe intermixing layer-induced competing effects of the compressed out-of-plane interplanarspacing of the constituent layers and free volume.
By using mechanical fatigue test associated with the in-situ measurement the change ofelectrical resistance method, the fatigue behavior of nanostructured Cu/X (X=Cr, Nb)multilayers was studied. The results show that a similar Coffin-Manson fatigue relationshipobserved commonly in bulk materials is found to be still operative in the multilayers,consisting with the results of Cu thin films. The suitable synergy between strength andductility can be achieved the maximum fatigue lifetime of thin film materials. Because thenucleation and motion of dislocations within the multilayers are strongly suppressed byincreased layer-to-layer interfaces, the fatigue damage of nanostructured Cu/X multilayers isboundary/interface dominated.
The length scale-dependent electric transport properties of nanostructured Cu/X (X=Cr, Nb)multilayers were measured using four-point probe technique. Both the theoretical analysisand experimental results show that the resistivity increases with decreasing the modulationperiod. The interface structure can remarkably influence the resistivity of nanostructuredCu/X multilayers. The best combination of mechanical-electrical properties can be achievedby artificially tailoring the microstructure of multilayers.
通过单轴拉伸和机械疲劳实验系统研究了介观尺度Cu薄膜的力学性能。结果表明，Cu薄膜的屈服强度以及疲劳行为（疲劳寿命与疲劳损伤）均表现出明显的尺寸依赖性。屈服强度以及疲劳寿命在某一临界尺寸下出现最大值。室温以及低应变速率下，纳米晶Cu薄膜呈现出变形孪晶的双反（晶粒）尺寸效应。根据经典的位错理论以及受激滑移模型，半定量解释了面心立方金属变形孪晶的双反（晶粒）尺寸效应。随着特征尺寸的减小，由于位错活动受到抑制以及可激活位错源的减少，疲劳损伤由位错滑移导致的挤出/侵入转变为与界面相关的损伤。
在单轴拉伸实验过程中利用薄膜电阻实时测量法，初步探索了不同体系Cu/X纳米多层膜的变形与断裂行为及其尺寸效应。研究发现，Cu/X纳米多层膜的屈服强度强烈依赖于其特征结构参数（调制周期与调制比），随调制周期的减小或者调制比的增加（即硬相体积分数增加）而增加，并伴随着变形机制的变化。这与通过约束层滑移模型和复合材料混合强度法则理论计算的结果相一致。由于软/延性相(Cu)对硬/脆性相(X)的异质约束作用，导致Cu/X纳米多层膜的延性以及断裂韧性随特征尺寸变化表现出奇异性，并且出现由张开型向剪切型断裂的转变。通过微观断裂力学模型定量阐述了软/延性相对硬/脆性相的约束作用对断裂行为的影响。此外，调制周期恒定的Cu/X纳米多层膜的强度与延性存在线性关系。界面约束越强（界面数量越多），线性关系的斜率越大。
纳米压痕实验揭示了界面结构对Cu/X (X=Cr、Nb)纳米多层膜的硬度及压入模量的影响。结果表明，Cu/X纳米多层膜的硬度呈现尺寸依赖性并随特征尺寸的减小达到饱和值，其变化趋势与屈服强度相同。与界面清晰的Cu/X多层膜单调变化的压入模量不同，界面混合（非晶）层导致Cu/X多层膜的压入模量出现最大值。通过考虑界面混合（非晶）层引起的组元层晶面间距压缩以及自由体积这两个竞争机制的相互作用，定性解释了压入模量的这种异常变化。
采用金属薄膜原位电阻变化法，通过机械疲劳试验研究了Cu薄膜和Cu/X (X=Cr、Nb)纳米多层膜的疲劳性能。结果表明，与块体材料相似，Cu/X纳米多层膜的疲劳寿命与应变幅仍然遵循经典的Coffin-Mason疲劳关系式，这与Cu薄膜是一致的。合理的强度和延性匹配能够实现薄膜材料疲劳性能的最优化。由于层间异质界面对位错活动的强烈抑制，Cu/X纳米多层膜的疲劳损伤由晶界/界面主导。
利用电阻四探针法系统研究了Cu/X (X=Cr、Nb)纳米多层膜的电输运行为及其尺寸效应。理论分析和实验结果均表明Cu/X纳米多层膜的电阻率均随着调制周期的减小而增加。界面结构可以显著影响纳米多层膜的电阻率。通过人工调控纳米多层膜的微观结构可以实现其力-电综合性能的最优化。
The single-/multi-layered films are widely used as essential components of high performancemicroelectronics, microelectromechanical systems and interconnect structures owing to theiroutstanding mechanical/electric properties. The deformation and fracture during themanufacture and service processes has been identified as an important factor influencingtheir reliability. The urgent demand for understanding the complex properties of thenanostructured multilayers and their constituent are both for scientific aspects and in theinterest of the engineering application. In this work, the mesoscaled mechanical/electronicproperties and the related physical mechanisms of nanocrystalline Cu films andnanostructured Cu/X (X=Cr, Nb, Zr) multilayers that typically used in microelectronicshave been investigated.
Uniaxial tensile test and mechanical fatigue test was respectively performed on themesoscaled Cu thin films to systemically investigate their mechanical properties. It isrevealed from the results that the yield strength of Cu thin films as well as the fatiguebehavior (fatigue lifetime and fatigue damage) is length scale-dependent. Maxima areobserved for both the yield strength and fatigue lifetime in mesoscaled Cu thin films at somecritical dimension. At room temperature and low strain rates, the nanocrystalline Cu thinfilms exhibit the double-inverse deformation twinning behavior with respect to the normalHall-Petch grain size dependence, which is semiquantitatively explained by the classicdislocation theory and dislocation stimulated slip model.With reducing the characteristicdimensions of Cu thin films, the fatigue damage of mesoscaled Cu thin films show thetransition from dislocation glide-induced extrusions/intrusions to boundary related damagedue to the inhibition of dislocation mobility and the limited availability and activation ofdislocation sources.
Uniaxial tensile test with combination of in-situ measurement the change of electricalresistance method was carried out to investigate the deformation and fracture behavior ofnanostructured Cu/X (X=Cr, Nb, Zr) multilayers. It is found that the yield strength of Cu/Xmultilayers strongly depends on the characteristic parameters (modulation period, λ andmodulation ratio, η), i.e., it increases with decreasing the modulation period or increasing themodulation ratio (or increasing the volume fraction of hard phase), accompanied with thetransition of deformation mechanism. This consists with the prediction by the confined layer slip model and the rule of mixture. Due to the constraint effects of soft/ductile phase (Cu) onhard/brittle phase (X), the nanostructured Cu/X multilayers present singularity ductility aswell as fracture toughness, and also show the transition of fracture mode from shearing toopening related to the length scale. The fracture behavior in Cu/X multilayers isquantitatively assessed using a fracture mechanism-based micromechanical model. Moreover,at a constant modulation period, Cu/X multilayers exhibit ductility scaling linearly with yieldstrength that is varied with modulation ratio. The scaling slope for Cu/X multilayers withmore interfaces is much sharper than that of ones with fewer interfaces, owing to a strongerinterface constraint caused by more interfaces.
The nanoindentation test was adopted to explore the effect of interface structure ofnanostructured Cu/X (X=Cr, Nb) multilayers on hardness and modulus. It is revealed thatthe hardness is also length scale-dependent, similar to that of yield strength. Different fromthe monotonic modulation period dependence known for Cu/X multilayers with clearinterface, a maximum indentation modulus is found in the Cu/X multilayers with theinterfacial intermixing (amorphous) layer. This unusual behavior is explained by consideringthe intermixing layer-induced competing effects of the compressed out-of-plane interplanarspacing of the constituent layers and free volume.
By using mechanical fatigue test associated with the in-situ measurement the change ofelectrical resistance method, the fatigue behavior of nanostructured Cu/X (X=Cr, Nb)multilayers was studied. The results show that a similar Coffin-Manson fatigue relationshipobserved commonly in bulk materials is found to be still operative in the multilayers,consisting with the results of Cu thin films. The suitable synergy between strength andductility can be achieved the maximum fatigue lifetime of thin film materials. Because thenucleation and motion of dislocations within the multilayers are strongly suppressed byincreased layer-to-layer interfaces, the fatigue damage of nanostructured Cu/X multilayers isboundary/interface dominated.
The length scale-dependent electric transport properties of nanostructured Cu/X (X=Cr, Nb)multilayers were measured using four-point probe technique. Both the theoretical analysisand experimental results show that the resistivity increases with decreasing the modulationperiod. The interface structure can remarkably influence the resistivity of nanostructuredCu/X multilayers. The best combination of mechanical-electrical properties can be achievedby artificially tailoring the microstructure of multilayers.
引文
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