Phase stability in metallic multilayers

As the thin film materials used in electronic and optical applications continue to decrease in thickness to the nano-scales, marked changes in functional properties are expected to occur due to changes in crystal structure of these materials. Therefore, such multilayer systems have been of considerable interest due to the ability to control properties by engineering the structure of materials at these scales. The new characterization tools allow direct imaging and analysis of such materials in order to link the performance variations with the crystal structure variations.; Transmission Electron Microscopy (TEM) has been often the technique of choice in characterization of nanomaterials enabling not only imaging the structure of the material but also chemically probing of the composition changes at a high spatial resolution. The ultimate resolution achievable in the electron microscope is a product of both microscope and the specimen and the simultaneous effect of each defines the quality and quantity of the information transferred through the microscope. In this sense, the common ion-beam assisted TEM sample preparation techniques have been deeply recognized as being surface damaging at high ion milling energies (>5kV) thus limiting the information transfer in the microscope. For the first time, a low energy (<2kV) focused Ar ion beam milling system has been applied to remove the surface artifacts created by the high energy conventional broad Ar or focused Ga beam milling techniques. The overall quality of the samples drastically improved after the application of the low energy milling practices and the outcome results directly enhanced the clarity of the information gathered at the atomic and nanoscale by the electron microscope.; Besides the specimen the resolution achievable in the electron microscope is strongly limited by the imperfections in the electron optics of the microscope column such as the spherical aberration of the electromagnetic lenses. Recently this problem has been solved by the correction of the spherical aberration of the microscope using a set of non-round lenses and consequently the information limit in an aberration corrected microscope (<0.1nm) has been pushed beyond an uncorrected microscope (∼0.13nm). In 2007, such a corrector system in the probe-forming lens of a Scanning TEM microscope was successfully installed at The Ohio State University. The preliminary results from this microscope were presented in the content of this work where we have studied the microscope and performed first hand experiments.; Finally we have addressed the phase stability in Cu/Nb and Ti/Nb nanoscale metallic multilayers by extensive use of these advance characterization techniques and tools. At reduced layer thickness (<2nm) the change in fcc to bcc phase in Cu and hcp to bcc phase in Ti were experimentally confirmed using X-ray diffraction electron diffraction and electron imaging techniques along the plan-view and cross-section directions. These structural transformations were often referred to as being thermodynamic in nature and a classical thermodynamical model explains and predicts the formation of such pseudomorphic phases through the competition of volumetric and interfacial free energy variables. We have investigated both the structural and chemical changes in the Cu/Nb and Ti/Nb nanoscale metallic mutilayers as a function of length scale in order to understand and predict the phase stability. The important constituents: volumetric free energy and interfacial energy changes were experimentally derived considering the chemistry and structure of the multilayers and competition between these thermodynamic terms well explains the observed structural changes in nanoscale metallic multilayers.