Publications

Interfacial adhesion is of extraordinary technological importance and has long been of intense scientific interest. However, the study of the adhesive bond and its failure is made difficult by the complexity of the interfacial interaction and the problems involved with establishing carefully characterized and controlled interfacial surfaces and that of quantitatively evaluating the bonding after its formation. In the present work, we outline the results of studies using Interfacial Force Microscopy (IFM) to study the adhesive bond formation and failure between (1) differing end-group combinations on self-assembling monolayer (SAM) films covering Au surfaces and (2) between clean surfaces of a W probe and a Au single-crystal sample. The IFM is a scanning probe technique distinguished by its use of a mechanically stable, zero-compliance force sensor. This sensor permits the study of the interfacial force as a function of separation without the mechanical instability giving rise to the {open_quotes}jump-to-contact{close_quotes} seen in all presently used displacement-based sensors, such as the surface forces apparatus and the atomic force microscope. Thus, information can be obtained concerning the details of the adhesive bond formation and failure over the entire range of the interfacial interaction. We demonstrate that such measurements yield valuable quantitative information concerning the individual bond strengths between chemically distinct SAM end groups and show that the clean metal-surface interaction is dominated by surface roughness and plastic deformation.

The capabilities of Interfacial Force Microscopy (IFM) are illustrated utilizing the following examples: the bonding interaction between chemically distinct end groups on self-assembling molecules adsorbed on the sample and and probe tip; and a study of the effect of morphological defects on the nanomechanical properties of gold single crystal surfaces.

The scanning force microscopies (notably the Atomic Force Microscope--AFM), because of their applicability to nearly all materials, are presently the most widely used of the scanning-probe techniques. However, the AFM uses a deflection sensor to measure sample/probe forces which suffers from an inherent mechanical instability that occurs when the rate of change of the force with respect to the interfacial separation becomes equal to the spring constant of the deflecting member. This instability dramatically limits the breadth of applicability of AFM-type techniques to materials problems. In the course of implementing a DOE sponsored basic research program in interfacial adhesion, a self-balancing force sensor concept has been developed and incorporated into an Interfacial Force Microscopy (IFM) system by Sandia scientists. This sensor eliminates the instability problem and greatly enhances the applicability of the scanning force-probe technique to a broader range of materials and materials parameters. The impact of this Sandia development was recognized in 1993 by a Department of Energy award for potential impact on DOE programs and by an R and D 100 award for one of the most important new products of 1994. However, in its present stage of development, the IFM is strictly a research-level tool and a CRADA was initiated in order to bring this sensor technology into wide-spread availability by making it accessible in the form of a commercial instrument. The present report described the goals, approach and results of this CRADA effort.

Stress in thin films plays a critical role in many technologically important areas. The role is a beneficial one in strained layer superlattices where semiconductor electrical and optical properties can be tailored with film stress. On the negative side, residual stress in thin-film interconnects in microelectronics can lead to cracking and delamination. In spite of their importance, however, surface and thin-film stresses are difficult to measure and control, especially on a local level. In recent studies, we used the Interfacial Force Microscope (IFM) in a nanoindenter mode to survey the nanomechanical properties of Au films grown on various substrates. Quantitative tabulations of the indentation modulus and the maximum shear stress at the plastic threshold showed consistent values over individual samples but a wide variation from substrate to substrate. These values were compared with film properties such as surface roughness, average grain size and interfacial adhesion and no correlation was found. However, in a subsequent analysis of the results, we found consistencies which support the integrity of the data and point to the fact that the results are sensitive to some property of the various film/substrate combinations. In recent measurements on two of the original substrate materials we found a direct correlation between the nanomechanical values and the residual stress in the films, as measured globally by a wafer warping technique. In the present paper, we review these earlier results and show recent measurements dealing with stresses externally applied to the films which supports our earlier conclusion concerning the role of stress on our measurements. In addition, we present very recent results concerning morphological effects on nanomechanical properties which add additional support to the suggestion that near-threshold indentation holds promise of being able to measure stress on a very local level.

In recent studies, we used the Interfacial Force Microscope in a nanoindenter mode to survey the nanomechanical properties of Au films grown on various substrates. Quantitative tabulations of the indentation modulus and the maximum shear stress at the plastic threshold showed consistent values over individual samples but a wide variation from substrate to substrate. These values were compared with film properties such as the surface roughness, average grain size and interfacial adhesion and no correlation was found. However, in a subsequent analysis of the results, we found consistencies which support the integrity of the data and point to the fact that the results are sensitive to some property of the various film/substrate combinations. In the present paper, we discuss these consistencies and show recent measurements which strongly suggest that the property that is being probed is the residual stress in the films caused by their interaction with the substrate surfaces.

This report summarizes research on the aging of Class I components in environments representative of nuclear power plants. It discusses Class IE equipment used in nuclear power plants, typical environments encountered by Class IE components, and aging techniques used to qualify this equipment. General discussions of radiation chemistry of polymers and accelerated aging techniques are also included. Based on the inadequacies of present aging techniques for Class IE equipment, a proposal for an experimental program on electrical cables is presented. One of the main purposes of the proposed work is to obtain relevant data in two areas of particular concern--the effect of radiation dose rate on polymer degradation, and the importance of synergism for combined thermal and radiation environments. A new model that allows combined environment accelerated aging to be carried out is introduced, and it is shown how the experimental data to be generated can be used to test this model.