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We investigated the process of the hole inlet closure in surface-diffusion-driven transformation of arrays of high-aspect-ratio holes on Si(001) substrates. The inlet gradually shrinks while keeping the circular shape because of lateral bulging of the inlet surface. We observed complicated top view morphologies reflecting the four-fold symmetry of the Si(001) surface on the inlet surface. Large {111} and {113} facets are formed in the four equivalent azimuths of the [110], while corrugated patterns arise in the four equivalent azimuths of the [100]. Atomic force microscopy observations reveal that the corrugated pattern is composed of three types of small facets, namely, {110} and two {113} in relation of the mirror symmetry. The corrugated pattern formation is due to the geometrical restriction that there is no stable facet between (001) and (010) in the [010] azimuth. The observed morphological evolution is interpreted as surface-diffusion-driven transformation under constraint of the anisotropic surface energy of Si.

High-temperature silicon dioxide chemical vapor deposition (HTOCVD), using SiH2Cl2 and N2O, can realize dense and conformal oxide film, not only on large size silicon wafers, but even inside of microscopic silicon trenches, at high-temperature around 800°C.In this work, we investigated the kinetics of HTOCVD using a commercial scale low pressure (LP) CVD reactor, focusing on the correlation between deposition rate and surface-to-volume ratio (S/V ratio), which is a specific surface area of substrate wafer divided by the space volume between two adjacent wafers. We also investigated the deposition rate profile on wafers, and along the axial direction of the reactor near the region where one, two or three substrate wafers are extracted from the quartz holder. The deposition rate profiles on wafer characteristically change from skillet-like to pancake-like, according to the increase of wafer spacing. The influence on the deposition rate of wafer spacing spreads to ranges not only downstream, but also upstream in the gas flow. These experimental results strongly suggest that in the HTOCVD gas-phase reactions through intermediate states of active species contribute to deposition reaction as well as direct deposition reaction of source gases on Si surface.

We have developed an atomic force microscopy (AFM) observation technique with which Si trench sidewall surface can be scanned with the tip of cantilever to investigate its nano-scale morphologies. By developing a new technique of cleaving the substrate at the center of a micron-sized trench along its longitudinal direction [011], the sidewall nano-scale morphology of the trench could be observed with the AFM technique. By comparing of cross sections of the images, we also investigated the difference between Si and carbon nanotube (CNT) tips for the AFM observations. According to the results, the CNT tip proved to show a superior signal-to-noise (S/N) ratio compared with the Si tip. The CNT tip enables us to observe the step patterns of the sidewalls of micron-sized trench structures in the various phases of hydrogen annealing.

We have examined how the morphology of the trench sidewall evolves in the early phase of hydrogen annealing under the two conditions of hydrogen pressures. A distinguished result was obtained concerning the sidewall surface morphology after 30 s annealing at 1000 °C under 760 Torr hydrogen ambient. The evanescence of chemical Si dioxide formed by RCA cleaning process was clearly observed to initiate in various places on the surface. And in the area without chemical oxide, the appearance of atomic steps was also observed. In contrast under 40 Torr hydrogen ambient, the chemical oxide was completely removed even after 30 s annealing. Our observation shows that not only the rate of trench shape transformation but also the rate of removal of oxide films decreases with increasing hydrogen pressure.

Thickness uniformities of poly-crystalline silicon thin films, deposited by a commercial LPCVD reactor, were investigated through a phenomenological and elementary reaction analysis. To understand the deposition rate and its profile in radius direction of ø 6”h silicon wafer, concentration distributions of film precursors were examined by solving basic diffusion equations of film precursors in the CVD system. The experimental thickness distribution can be simulated very well with the solution by optimizing η, the sticking probabilities of the precursors. While most of the silicon deposition was made by source precursor (mono-silane, SiH4), two kinds of intermediate species with sticking probabilities of 5X10-2 and 7X10-4 were found to contribute the deposition. Subsequently, elementary chemical reaction analysis of poly-crystalline silicon CVD process was performed using ChemKinTM and two chemical species, SiH2 and Si2H6, were identified as the possible candidates for the intermediate species.

Nanolithography has been studied by using electron beam technology. Ten-nm linewidth PMMA resist patterns have been demonstrated by 50 kV scanning electron beam. The self-developing properties of a AlF3 doped LiF inorganic resist under a scanning electron beam irradiation with energy of 20–50 keV have been studied for sub-10 nm lithography. By optimizing the inorganic resist film quality, 5 nm linewidth patterns with 60 nm periodicity were directly delineated under a 30 keV electron beam. Another approach for nanolithography using electron beam holography has been proposed. Line and dot patterns with 100 nm periodicity were exposed on PMMA resist by electron beam holography with thermal field emitter gun and an electron biprism. Subsequent atomic force microscope observation has confirmed that both patterns are successfully fabricated. This technique allows us to produce nanoscale periodic patterns simultaneously. The selective atomic desorption of Cl atoms adsorbed on a Si (111) 7×7 surface has been studied by field evaporation using a scanning tunneling microscope (STM). The STM tip is placed on the adsorbed Cl on the surface, and pulse voltage was applied. This results in selective atomic desorption of Cl.