A team of researchers at Aix Marseille Université in Marseille, France, led by Frédéric Leroy, has developed a technique that allows them to follow atomic-scale physical processes occurring at the surfaces of materials in situ and in real time.

With this new technique, which is based on the principles of electron microscopy, the research team were able to study the kinetics of decomposition of a thin layer of silicon dioxide deposited onto silicon during a thermal treatment, a critical component in micro-electronics. This work is reported in a paper in Applied Physics Letters.

Silicon dioxide (SiO2) is one of the most important building blocks of micro-electronics and its thermal stability is critical to device performance. The decomposition of a thin layer of silicon dioxide onto silicon has thus been the focus of a great deal of scientific interest for four decades. Previous studies have shown that the decomposition occurs non-homogeneously at the surface via the local formation of holes in the oxide layer that extend laterally.

Understanding the elementary atomic processes responsible for the opening velocity of these holes is essential for improving the performance of silicon dioxide, and required the development of advanced characterization tools.

"We needed to be able to characterize the structural (crystallography, size, shape) and the chemical properties at the same time and to be able to follow in situ and in real time the changes during a given process for a rapid feedback on the experimental parameters," Leroy explained. "Our approach based on low-energy electron microscopy is the cornerstone of our achievements."

"It was impossible to adjust all control parameters of the electron microscope before the decomposition process started since silicon dioxide is amorphous, so we had to adjust finely the settings within a few seconds as soon as the oxide decomposes in order to characterize the whole process."Frédéric Leroy, Aix Marseille Université

Even with their new instrument, however, the team encountered challenges. Obtaining real time measurements of the thermal decomposition of the silicon dioxide was particularly difficult since the complete process occurs in just a few minutes in a narrow temperature window.

"It was impossible to adjust all control parameters of the electron microscope before the decomposition process started since silicon dioxide is amorphous, so we had to adjust finely the settings within a few seconds as soon as the oxide decomposes in order to characterize the whole process," Leroy explained.

This meticulous measurement yielded some surprising results. Leroy and his research team found experimental evidence that the decomposition process was not initially in a steady state regime, as previous studies had argued.

"Our results imply that the conventional view of a steady state regime for the silicon dioxide decomposition related to a simplified reaction Si+SiO2-> 2SiO(g) occurring at the hole edge is not generally true," Leroy said. Instead, the team's results imply that silicon dioxide decomposition occurs via hole nucleation and opening with a circular shape.

The velocity of hole opening is intimately related to the decomposition rate of silicon dioxide at the periphery of the holes. Initially, large holes open quickly thanks to a chemical reaction catalyzed by molecular species such as silicon hydroxyls present inside the hole. Researchers suspect these species agglomerate during long thermal annealing and are released inside the holes during the silicon dioxide decomposition.

The main applications of this work are in micro-electronics, particularly all steps of thermal treatments. "We have shown that the silicon dioxide formed by a wet chemical treatment is highly defective after a long thermal annealing," Leroy said. "The next step in our research is to study the interplay between chemical reactions and the enhancement of the mobility of nanostructures."

This story is adapted from material from the American Institute of Physics, with editorial changes made by Materials Today. The views expressed in this article do not necessarily represent those of Elsevier. Link to original source.