In Situ and Real-Time Nanoscale Monitoring of Ultra-Thin Metal Film Growth Using Optical and Electrical Diagnostic Tools

Continued downscaling of functional layers for key enabling devices has prompted the development of characterization tools to probe and dynamically control thin film formation stages and ensure the desired film morphology and functionalities in terms of, e.g., layer surface smoothness or electrical properties. In this work, we review the combined use of in situ and real-time optical (wafer curvature, spectroscopic ellipsometry) and electrical probes for gaining insights into the early growth stages of magnetron-sputter-deposited films. Data are reported for a large variety of metals characterized by different atomic mobilities and interface reactivities. For fcc noble-metal films (Ag, Cu, Pd) exhibiting a pronounced three-dimensional growth on weakly-interacting substrates (SiO2, amorphous carbon (a-C)), wafer curvature, spectroscopic ellipsometry, and resistivity techniques are shown to be complementary in studying the morphological evolution of discontinuous layers, and determining the percolation threshold and the onset of continuous film formation. The influence of growth kinetics (in terms of intrinsic atomic mobility, substrate temperature, deposition rate, deposition flux temporal profile) and the effect of deposited energy (through changes in working pressure or bias voltage) on the various morphological transition thicknesses is critically examined. For bcc transition metals, like Fe and Mo deposited on a-Si, in situ and real-time growth monitoring data exhibit transient features at a critical layer thickness of ~2 nm, which is a fingerprint of an interface-mediated crystalline-to-amorphous phase transition, while such behavior is not observed for Ta films that crystallize into their metastable tetragonal β-Ta allotropic phase. The potential of optical and electrical diagnostic tools is also explored to reveal complex interfacial reactions and their effect on growth of Pd films on a-Si or a-Ge interlayers. For all case studies presented in the article, in situ data are complemented with and benchmarked against ex situ structural and morphological analyses.

Determination of Stresses in Incrementally Deposited Films From Wafer-Curvature Measurements

We report closed-form formulas to calculate the incremental-deposition stress, the elastic relaxation stress, and the residual stress in a finite-thickness film from a wafer-curvature measurement. The calculation shows how the incremental deposition of a new stressed layer to the film affects the amount of the film/wafer curvature and the stress state of the previously deposited layers. The formulas allow the incremental-deposition stress and the elastic relaxation to be correctly calculated from the slope of the measured curvature versus thickness for arbitrary thicknesses and biaxial moduli of the film and the substrate. Subtraction of the cumulative elastic relaxation from the incremental-deposition stress history results in the residual stress left in the film after the whole deposition process. The validities of the formulas are confirmed by curvature measurements of electrodeposited Ni films on substrates with different thicknesses.

Mechanical, thermal, and electrochemical properties of Pr doped ceria from wafer curvature measurements

This work demonstrates, for the first time, that a variety of disparate and technologically-relevent thermal, mechanical, and electrochemical oxygen-exchange material properties can all be obtained from in situ, current-collector-free wafer curvature measurements.