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The growth mechanism of the prototypical atomic layer deposition (ALD) process of Al2O3 using Al(CH3)3 (TMA) and H2O has been revisited on the basis of insights obtained with the nonlinear optical analysis technique of broadband sum-frequency generation (BB-SFG). With BB-SFG spectroscopy, both the –CH3 and –OH surface groups ruling the growth of Al2O3 by ALD were detected and could be monitored during the ALD process with submonolayer sensitivity. Several remaining questions pertaining to the growth mechanism of Al2O3 were addressed. The reaction kinetics of the H2O half-cycle were studied for ALD between 100 and 300 °C, and the reaction cross section σ was determined. The cross section at 300 °C was fairly large (σ = 3 × 10−19 cm2) and it decreased with decreasing temperature. Below 200 °C, the cross section also clearly varied with the surface coverage. For example, at 100 °C, the cross section started at σ = 1 × 10−20 cm2 for a full –CH3 coverage and decreased to σ = 3 × 10−21 cm2 for a 60% coverage. T...

Revisiting the growth mechanism of atomic layer deposition of Al2O3: A vibrational sum-frequency generation study