Plasma Anneal As a Stress Control Method in Low Temperature Al2O3 ALD Coatings

Abstract

The control of mechanical physical stress is an important requirement in a variety of applications, such as flexible electronics or thick optical coatings where film stress can cause delamination. Traditionally, in thermal ALD it has been difficult to control the stress. Al2O3 deposited at low temperature is consistently found to have a tensile stress level in the range of a 300 to 450 MPa ( refs 1-3). It is well established that In magnetron sputtering , film stress can be controlled straightforwardly using the Argon pressure during deposition, as this affects the level of bombardment of the growing film with energetic particles.Paranjpe et al ( ref 1) have demonstrated that the use of a plasma anneal leads to densification and transition of the stress from tensile to compressive. The process consists of a sequence of deposition of a thin layer ( e.g. 5 nm) by thermal ALD, followed by exposure to a low energy plasma. The atomic displacements caused by low energy ions from the plasma tend to lead to filling of nanoscopic voids and point defects, thus releasing tensile stress.In this presentation, we will review an in depth study of the effect of various process parameters on the ability of a capacitively coupled in-situ plasma anneal to control stress. The following parameters will be reviewed: Gas composition: Argon plasmas, Oxygen plasmas and Argon oxygen mixtures are compared. Gas Pressure: The effect of gas pressure on plasma characteristics and the resulting modification of the coating is studied RF Power: RF Power was varied between 0 and 300 W ( 1.32 W/cm2) Plasma duration : The duration of the plasma treatment was varied from 0 to 60 seconds.A process window was identified where the plasma anneal can be used as an effective, controllable tool to reduce stress in the coatings. This is illustrated in fig. 1, which shows the substrate warpage (“bow”) observed in 75 mm thick PET foils with a 50 nm Al2O3 coating deposited at 90 °C. It can be seen that the untreated coating (0 sec plasma) has a bow corresponding to a tensile stress of 370 MPa, in accordance with literature values. As the plasma anneal time increases, the stress value decreases. Applying a 60 sec plasma every 5 nm allows to deposit a virtually stress free coating. Simultaneously with the stress reduction, an increase of the optical index and a slight reduction of the thickness are observed, consistent with a densification of the coating.