Quantitative and nondestructive determination of residual stress for SiO2 thin film by laser-generated surface acoustic wave technique

The laser-generated surface acoustic wave (SAW) technique is a promising method to measure the mechanical properties of thin films quickly and nondestructively. Residual stress is inevitable during the processing and manufacturing of integrated circuits, which will have a major impact on the physical and mechanical properties of the thin film materials and cause deterioration to the structural strength. In this study, the SAW technique based method is proposed for quantitative and nondestructive measuring the residual stress in the nanostructured films. The method is verified by the experiment measuring the SiO2 films in the thickness range of 100 to 2000 nm. The experimental procedures, including signal excitation, reception and processing, are described in detail. By matching the SAW experimental dispersion curve with the calculated theoretical dispersion curve containing the residual stress, the residual stress of the SiO2 films along [110] and [100] crystallographic orientation of the Si wafer is successfully quantified. The determination results are ranged from -65.5 to 421.1 MPa and the stress value increases as the film thickness decreases, revealing the residual stress of the SiO2 film is compressive. Meanwhile, the conventional substrate curvature method as a comparison is used to verify the correctness and feasibility of the proposed SAW method for the residual stress determination.

Preparation of High-Transparency, Superhydrophilic Visible Photo-Induced Photocatalytic Film via a Rapid Plasma-Modification Process

In this study, different amounts of SiO2 nanoparticles (7 nm) were added to simultaneously reach high transmittance, high hardness, and high adhesion for TiO2 film prepared by the sol–gel method and coated on glass through a dip-coating technique. For the film to achieve self-cleaning, anti-fogging, superhydrophilicity, and visible photo-induced photocatalysis, TiO2-SiO2 film was modified via a rapid microwave plasma-nitridation process for efficient N-doping by various N2-containing gases (N2, N2/Ar/O2, N2/Ar). Through nitrogen plasma, the content of N atom reached 1.3% with the ratio of O/Ti atom being 2.04. The surface of the thin films was smooth, homogeneous, and did not crack, demonstrated by the root mean square (RMS) roughness of film surface being 3.29–3.94 nm. In addition, the films were composed of nanoparticles smaller than 10 nm, with a thickness of about 100 nm, as well as the crystal phase of the thin film being anatase. After the plasma-nitridation process, the visible-light transmittance of N-doped TiO2-SiO2 films was 89.7% (clean glass = 90.1%). Moreover, the anti-fogging ability was excellent (contact angle < 5°) even without light irradiation. The degradation of methylene blue showed that the photocatalytic performance of N-doped TiO2-SiO2 films was apparently superior to that of unmodified films under visible-light irradiation. Moreover, the pencil hardness and adhesion rating test of the thin films were 7H and 5B, respectively, indicating that the obtained coatings had great mechanical stability.

Deposition and Characterization of RP-ALD SiO2 Thin Films with Different Oxygen Plasma Powers

In this study, silicon oxide (SiO2) films were deposited by remote plasma atomic layer deposition with Bis(diethylamino)silane (BDEAS) and an oxygen/argon mixture as the precursors. Oxygen plasma powers play a key role in the quality of SiO2 films. Post-annealing was performed in the air at different temperatures for 1 h. The effects of oxygen plasma powers from 1000 W to 3000 W on the properties of the SiO2 thin films were investigated. The experimental results demonstrated that the SiO2 thin film growth per cycle was greatly affected by the O2 plasma power. Atomic force microscope (AFM) and conductive AFM tests show that the surface of the SiO2 thin films, with different O2 plasma powers, is relatively smooth and the films all present favorable insulation properties. The water contact angle (WCA) of the SiO2 thin film deposited at the power of 1500 W is higher than that of other WCAs of SiO2 films deposited at other plasma powers, indicating that it is less hydrophilic. This phenomenon is more likely to be associated with a smaller bonding energy, which is consistent with the result obtained by Fourier transformation infrared spectroscopy. In addition, the influence of post-annealing temperature on the quality of the SiO2 thin films was also investigated. As the annealing temperature increases, the SiO2 thin film becomes denser, leading to a higher refractive index and a lower etch rate.