Effects of adhesion on the measurement of thin film mechanical properties by nanoindentation

Experiments have been performed on soft aluminum films deposited on hard ceramic substrates to explore the influences of interfacial adhesion on mechanical property measurement by nanoindentation. The substrate materials included soda-lime silicate glass, aluminum oxynitride (ALON), and (100) sapphire. Thin films of high purity aluminum were sputtered onto each substrate to a thickness of 500 nm. Because the films were deposited simultaneously, the only major difference in the specimens was the nature of the substrate, which exerts an important influence on film adhesion through interfacial chemistry. Of the substrates examined, aluminum adheres strongly to glass and sapphire, but poorly to ALON. In addition, two different types of aluminum films on sapphire were examined - one with and the other without a 10 nm interlayer of amorphous carbon which significantly reduces film adhesion. Testing revealed important differences in the hardness of the specimens when measured by standard nanoindentation methods. Characterization of the residual hardness impressions by high resolution scanning electron microscopy showed that the hardness differences arise from an influence of interfacial debonding and film delamination on pile-up in the film. Furthermore, when the pile-up is accounted for in contact area determinations, the film hardness is actually independent of the substrate, thus indicating that the hardness differences observed in nanoindentation testing are an artifact of the testing analysis procedure. Results of the experiments are documented and discussed. 8 refs., 6 figs., 1 tab

Nanoindentation hardness of soft films on hard substrates: Effects of the substrate

The ability to accurately measure the mechanical properties of thin metallic films is important in the semiconductor industry as it relates to device reliability issues. One popular technique for measuring thin film mechanical properties is nanoindentation. This technique has the advantage of being able to measure properties such as hardness and elastic modulus without removing a film from its substrate. However, according to a widely-held rule of thumb, intrinsic film properties can be measured in a manner which is not influenced by the substrate only if the indentation depth is kept to less than 10% of the film thickness, which is often not practical. In this work, a method for making substrate independent hardness measurements of soft metallic films on hard substrates is proposed. The primary issue to be addressed is the substrate-induced enhancement of indentation pile-up and the ways in which this pile-up influences the contact area determined from analyses of nanoindentation load- displacement data. Based on experimental observations of soft aluminum films on silicon, glass, and sapphire substrates, a simple empirical relationship is derived which relates the amount of pile-up to the contact depth. From this relationship, a simple method is developed which allows the intrinsic hardness of the film to be measured by nanoindentation methods even when the indenter penetrates through the film into the substrate

Nanoindentation of soft films on hard substrates: The importance of pile-up

Nanoindentation is used for measuring mechanical properties of thin films. This paper addresses potential measurement errors caused by pile-up when soft films deposited on hard substrates are tested this way. Pile-up is exacerbated in soft film/hard substrate systems because of the constraint the substrate exerts on plastic deformation of the film. To examine pile-up effects, Al films 240 and 1700 nm thick were deposited on hard glass and tested by standard nanoindentation. In Al/glass, the film and substrate have similar elastic moduli; thus, any unusual behavior in nanoindentation results may be attributed to differences in plastic flow alone. SEM examination of nanoindentation hardness impressions in the film revealed that common methods for analyzing nanoindentation data underestimate the true contact areas by as much as 80%, which results in overestimations of the hardness and modulus by as much as 80 and 35%, respectively. Sources of these errors and their effect on measurement of hardness and elastic modulus are discussed, and a simple model for the composite hardness of the film/substrate system is developed. This model could prove useful when it is not possible to make indentations shallow enough to avoid substrate effects

Nanoindentation of soft films on hard substrates: Experiments and finite element simulations

Experiments and finite element simulations have been performed to examine error measurement of hardness and elastic modulus caused by pile-up when soft films deposited on hard substrates are tested by nanoindentation methods. Pile-up is exacerbated in soft-film/hard-substrate systems by the constraint imposed on plastic deformation in the film by the relatively non-deformable substrate. To experimentally examine pile-up effects, soft aluminum films with thicknesses of 240, 650, and 1700 nm were deposited on hard soda-lime glass substrates and tested by nanoindentation techniques. This system is attractive because the elastic modulus of the film and the substrate are approximately the same, but the substrate is harder than the film by a factor of about ten. Consequently, substrate influences on the indentation load-displacement behavior are manifested primarily by differences in the plastic flow characteristics alone. The elastic modulus of the film/substrate system, as measured by nanoindentation techniques, exhibits an increase with indenter penetration depth which peaks at a value approximately 30% greater than the true film modulus at a penetration depth close to the film thickness. Finite element simulation shows that this unusual behavior is caused by substrate-induced enhancement of pile-up. Finite element simulation also shows that the amount of pile-up increases with increasing penetration depth, and that the pile-up geometry depends on the work-hardening characteristics of the film. Because of these effects, nanoindentation techniques overestimate the true film hardness and elastic modulus by as much as 68% and 35%, respectively, depending on the work-hardening behavior of the film and the indenter penetration depth. The largest errors occur in non-work-hardening materials at penetration depths close to the film thickness, for which substrate-induced enhancement of pile-up is greatest