RESUMEN
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 ß-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.
RESUMEN
Synchrotron experiments combining real-time stress, X-ray diffraction, and X-ray reflectivity measurements, complemented by in situ electron diffraction and photon electron spectroscopy measurements, revealed a detailed picture of the interfacial silicide formation during deposition of ultrathin Pd layers on amorphous silicon. Initially, an amorphous Pd2Si interlayer is formed. At a critical thickness of 2.3 nm, this layer crystallizes and the resulting volume reduction leads to a tensile stress buildup. The [111] textured Pd2Si layer continues to grow up to a thickness of ≈3.7 nm and is subsequently covered by a Pd layer with [111] texture. The tensile stress relaxes already during Pd2Si growth. A comparison between the texture formation on SiOx and a-Si shows that the silicide layer serves as a template for the Pd layer, resulting in a surprisingly narrow texture of only 3° after 800 s Pd deposition. The texture formation of Pd and Pd2Si can be explained by the low lattice mismatch between Pd(111) and Pd2Si(111). The combined experimental results indicate a similar interface formation mechanism for Pd on a-Si and c-Si, whereas the resulting silicide texture depends on the Si surface. A new strain relaxation mechanism via grain boundary diffusion is proposed, taking into account the influence of the thickness-dependent crystallization on the material transport through the silicide layer. In combination with the small lattice mismatch, the grain boundary diffusion facilitates the growth of Pd clusters, explaining thus the well-defined thickness of the interfacial silicide layer, which limits the miniaturization of self-organized silicide layers for microelectronic devices.
RESUMEN
We report on a new route to grow epitaxial copper (Cu) ultra-thin films (up to 150 nm thick) at ambient temperature on Si(001) wafers covered with native oxide without any prior chemical etching or plasma cleaning of the substrate. It consists of a single-step deposition process using high power impulse magnetron sputtering (HiPIMS) and substrate biasing. For a direct current (DC) substrate bias voltage of -130 V, Cu/Si heteroepitaxial growth is achieved by HiPIMS following the Cu(001) [100]//Si(001) [110] orientation, while under the same average deposition conditions, but using conventional DC magnetron sputtering, polycrystalline Cu films with [111] preferred orientation are deposited. In addition, the intrinsic stress has been measured in situ during growth by real-time monitoring of the wafer curvature. For this particular HiPIMS case, the stress is slightly compressive (-0.1 GPa), but almost fully relaxes after growth is terminated. As a result of epitaxy, the Cu surface morphology exhibits a regular pattern consisting of square-shaped mounds with a lateral size of typically 150 nm. For all samples, X-ray diffraction pole figures and scanning/transmission electron microscopy reveal the formation of extensive twinning of the Cu {111} planes.
