Investigation of the Mechanical Properties of Thin Films by Nanoindentation, Considering the Effects of Thickness and Different Coating-Substrate Combinations

In order to further investigate nanoindentation data of film-substrate systems and to learn more about the mechanical properties of nanometer film-substrate systems, two kinds of films on different substrate systems have been tested with a systematic variation in film thickness and substrate characteristics. The two kinds of films are aluminum and tungsten, which have been sputtered on to glass and silicon substrates, respectively. Indentation experiments were performed with a Nano Indent XP II with indenter displacements typically about two times the nominal film thicknesses. The resulting data are analyzed in terms of load-displacement curves and various comparative parameters, such as hardness, Young's modulus, unloading stiffness and elastic recovery. Hardness and Young's modulus are investigated when the substrate effects are considered. The results show how the composite hardness and Young's modulus are different for different substrates, different films and different film thicknesses. An assumption of constant Young's modulus is used for the film-substrate system, in which the film and substrate have similar Young's moduli. Composite hardness obtained by the Joslin and Oliver method is compared with the directly measured hardness obtained by the Oliver and Pharr method.

The study on the interface adhesion comparison of the MgF2, Al2O3, SiO2 and Ag thin films

Adhesion between the interface of pure silver thin film and three kinds of low refractive index coatings MgF2, Al2O3, SiO2 were compared in this article. The results indicated that the adhesion of Al2O3 and Ag was evidently superior to that of MgF2 and Ag, and the adhesion of MgF2 and Ag was evidently superior to that Of SiO2 and Ag. Reasons were analyzed accordingly. On the other hand, we compared the effect on the optical characteristic of Ag film when these three kinds of films were used as protective coatings and enhanced coatings. Considering the difference of the adhesion between Ag and MgF2, Al2O3, SiO2, suited uses are given for each other. © 2004 Elsevier B.V. All rights reserved.

Thermodynamic damage mechanism of transparent films caused by a low-power laser

A new model for analyzing the laser-induced damage process is provided. In many damage pits, the melted residue can been found. This is evidence of the phase change of materials. Therefore the phase change of materials is incorporated into the mechanical damage mechanism of films. Three sequential stages are discussed: no phase change, liquid phase change, and gas phase change. To study the damage mechanism and process, two kinds of stress have been considered: thermal stress and deformation stress. The former is caused by the temperature gradient and the latter is caused by high-pressure drive deformation. The theory described can determine the size of the damage pit. (c) 2006 Optical Society of America.

Influence of oxygen partial pressure on the structure and photoluminescence of direct current reactive magnetron sputtering ZnO thin films

The effects of oxygen partial pressure on the structure and photoluminescence (PL) of ZnO films were studied. The films were prepared by direct current (DC) reactive magnetron sputtering with various oxygen concentrations at room temperature. With increasing oxygen ratio, the structure of films changes from zinc and zinc oxide phases, single-phase ZnO, to the (002) orientation, and the mechanical stresses exhibit from tensile stress to compressive stress. Films deposited at higher oxygen pressure show weaker emission intensities, which may result from the decrease of the oxygen vacancies and zinc interstitials in the film. This indicates that the emission in ZnO film originates from the oxygen vacancy and zinc interstitial-related defects. From optical transmittance spectra of ZnO films, the plasma edge shifts towards the shorter wavelength with the improvement of film stoichiometry. (C) 2004 Elsevier B.V. All rights reserved.

The effects of oxygen partial pressure on the optical absorption edge and the UV emission energy of ZnO films

The optical absorption edge and ultraviolet (UV) emission energy of ZnO films deposited by direct current (DC) reactive magnetron sputtering at room temperature have been investigated. With the oxygen ratio increasing, the structure of films changes from zinc and zinc oxide coexisting phase to single-phase ZnO and finally to the highly (002) orientation. Both the grain size and the stress of ZnO film vary with the oxygen partial pressure. Upon increasing the oxygen partial pressure in the growing ambient, the visible emission in the room-temperature photoluminescence spectra was suppressed without sacrificing the band-edge emission intensity in the ultraviolet region. The peaks of photoluminescence spectra were located at 3.06---3.15 eV. From optical transmittance spectra of ZnO films, the optical band gap edge was observed to shift towards shorter wavelength with the increase of oxygen partial pressure.

Thickness dependence of structure and optical properties of silver films deposited by magnetron sputtering

A series of silver films with different thickness were prepared under identical conditions by direct current magnetron sputtering. The optical properties of the silver films were measured using spectrophotometric techniques and the optical constants were calculated from reflection and transmission measurements made at near normal incidence. The results show that the optical properties and constants are affected by films' thickness. Below the critical thickness of 17 nm at which Ag film forms a continuous film, the optical properties and constants vary significantly as the thickness of films increases and then tends to a stable value which is reached at 41 nm. X-ray diffraction measurements were carried out to examine the structure and stress evolution of the Ag films as a function of films' thickness. It was found that the interplanar distance of (111) orientation decreases when the film thickness increases and tends to be close to that of bulk material. The compressive strains also decrease with increasing thickness. (C) 2007 Published by Elsevier B.V.

Influence of ytterbia content on residual stress and microstructure of Y2O3-ZrO2 thin films prepared by EB-PVD

Y2O3 stabilized ZrO2 (YSZ) thin films with different Y2O3 molar contents (0, 3, 7, and 12 mol%) are deposited on BK7 substrates by electron-beam evaporation technique. The effects of different Y2O3 contents on residual stresses and structures of YSZ thin films are studied. Residual stresses are investigated by means of two different techniques: the curvature measurement and x- ray diffraction method. It is found that the evolution of residual stresses of YSZ thin films by the two different methods is consistent. Residual stresses of films transform from compressive stress into tensile stress and the tensile stress increases monotonically with the increase of Y2O3 content. At the same time, the structures of these films change from the mixture of amorphous and monoclinic phases into high temperature cubic phase. The variations of residual stress correspond to the evolution of structures induced by adding of Y2O3 content.

High temperature annealing effect on structure, optical property and laser-induced damage threshold of Ta2O5 films

Ta2O5 films were deposited by conventional electron beam evaporation method and then annealed in air at different temperature from 873 to 1273 K. It was found that the film structure changed from amorphous phase to hexagonal phase when annealed at 1073 K, then transformed to orthorhombic phase after annealed at 1273 K. The transmittance was improved after annealed at 873 K, and it decreased as the annealing temperature increased further. The total integrated scattering (TIS) tests and AFM results showed that both scattering and root mean square (RMS) roughness of films increased with the annealing temperature increasing. X-ray photoelectron spectroscopy (XPS) analysis showed that the film obtained better stoichiometry and the O/Ta ratio increased to 2.50 after annealing. It was found that the laser-induced damage threshold (LIDT) increased to the maximum when annealed at 873 K, while it decreased when the annealing temperature increased further. Detailed damaged models dominated by different parameters during annealing were discussed. (C) 2008 Elsevier B. V. All rights reserved.

Low temperature annealing effects on the structure and optical properties of ZnO films grown by pulsed laser deposition

ZnO thin films were deposited on glass substrates at room temperature (RT) similar to 500 degrees C by pulsed laser deposition (PLD) technique and then were annealed at 150-450 degrees C in air. The effects of annealing temperature on the microstructure and optical properties of the thin films deposited at each substrate temperature were investigated by XRD, SEM, transmittance spectra, and photoluminescence (PL). The results showed that the c-axis orientation of ZnO thin films was not destroyed by annealing treatments: the grain size increased and stress relaxed for the films deposited at 200-500 degrees C, and thin films densified for the films deposited at RT with increasing annealing temperature. The transmittance spectra indicated that E-g of thin films showed a decreased trend with annealing temperature. From the PL measurements, there was a general trend, that is UV emission enhanced with lower annealing temperature and disappeared at higher annealing temperature for the films deposited at 200-500 degrees C; no UV emission was observed for the films deposited at RT regardless of annealing treatment. Improvement of grain size and stoichiometric ratio with annealing temperature can be attributed to the enhancement of UV emission, but the adsorbed oxygen species on the surface and grain boundary of films are thought to contribute the annihilation of UV emission. It seems that annealing at lower temperature in air is an effective method to improve the UV emission for thin films deposited on glass substrate at substrate temperature above RT.

Oriented growth and luminescence of ZnO : Eu films prepared by sol-gel process

A series of Eu3+-doped ZnO films have been prepared by a sol-gel method. These films were characterized by X-ray diffraction (XRD) and photoluminecent spectra (PL). Effects of synthetic parameters, such as annealing atmosphere, temperature and concentration of doped ions, on the highly oriented crystal growth were studied in detail. The crystalline structures of films annealed in vacuum have a wurtzite symmetry with highly c-axis orientation. A characteristic D-5(0) -> F-7(J)(J = 1, 2, 3 and 4) red emission is observed due to energy transfer from the ZnO host to the doped Eu3+ in the c-oriented ZnO films.

Studies on the morphology transition of micro-crystal growth in polymer films in high vacuum and strong electrostatic field

The morphology of films of isotactic polypropylene poly (3-dodecylthiophene) and iPP/P3DDT blend formed in electrostatic fields has been investigated by using scanning electron microscope. The experiment results show that the micro-crystal morphology of polymer films was strongly dependent on electrostatic fields. It was found that the effect of the electrostatic field led to the formation of dendrite crystals aligned in the field direction, and some branches of P3DDT ruptured. However, the micro-crystals in these films grew into spherulites without electrostatic field,and have no crystal orientation.

Femtosecond laser-induced crystallization in amorphous Ge2Sb2Te5 films

Crystallization in amorphous Ge2Sb2Te5 films by irradiation with femtosecond laser was investigated. The reflectivity and X-ray diffraction measurements confirmed that the crystalline state has been achieved in amorphous Ge2Sb2Te5 films under the irradiation of fermosecond laser with an average power of 65 mW at a frequency of 1000 Hz and a pulsed width of 120 fs. The surface morphology before and after femtosecond laser irradiation was studied by scanning electron microscope; results showed that the surface of films with irradiation of femtosecond laser was composed of some the crystallized micro-region. (C) 2004 Elsevier B.V. All rights reserved.

Photoinduced effects in amorphous Ge-Se films

With light illumination from an Ar ion laser, the photoinduced changes in vacuum evaporated amorphous GeSe2 films; were investigated with the X-ray diffraction (XRD), infrared absorption (IR), scanning electron microscope (SEM), transmitting electron microscope (TEM) and transmittance spectra analysis. It was observed that the optical transmittance edges of films shifted to shorter wavelength according to annealing and light illumination and the shift in well-annealed films could be recovered by annealing at 200 degrees C for 1 h in Ar air. The magnitude of shift increased with the increase of the intensity of illumination light and the illumination time. By sides, photoinduced crystallization was also observed in the exposed regions of GeSe2 films and more of it was observed with stronger intensity of illumination light.

Effect of processing parameters on the optical properties of TiO2/ormosil planar waveguide

Hybrid TiO2/ormosil waveguiding films have been prepared by the sol-gel method at low thermal treatment temperature of 150° C. The influence of processing parameters including the molar ratios of titanium butoxide (Ti(OBu)(4))/3-glycidoxypropyltrimethoxysilane (GLYMO) and H2O/Ti(OBu)(4) (expressed as R), especially aging of sot on the optical properties was investigated. The optical properties of films were measured with scanning electron microscope (SEM), UV/VIS/NIR spectrophotometer (UV-Vis), m-line and the scattering-detection method. The results indicate that the film thickness increases with the increase of sol aging time, but the variation of refractive index as a function of sot aging time depends on the relative ratios of GLYMO to Ti(OBu)(4). Higher transmittance and lower attenuation of the planar waveguide can be obtained in the sol with lower Ti(OBu)(4) contents and shorter aging time.

Optical and surface properties of hybrid TiO2/ormosil planar waveguide prepared by the sol-gel process

Two kinds of silanes, 3-glycidoxypropyltrimethoxysilane (GLYMO) and 3-trimethoxysililpropylmethacrylate (TMSPM), were used to prepare ormosil waveguide films by the sol-gel method. Thirty percent Ti(OBu)(4) and 70% silane were contained in the precursor sets. The properties of films were measured by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV/VIS/NIR spectrophotometer (UV-vis), atomic force microscopy (AFM), m-line and scattering-detection method. The films from GLYMO and TMSPM precursors exhibit similar thickness (2.58 mu m for GLYMO, 2.51 mu m for TMSPM) and refractive index (1.5438 for GLYMO, 1.5392 for TMSPM, lambda=632.8 nm), but the film from TMSPM precursor has higher propagation loss (1.024 dB/cm, lambda=632.8 nm) than the film prepared from GLYMO (0.569 dB/cm, lambda=632.8 nm). Furthermore, the film prepared from TMSPM is easy to be opaque and cracks during coating whereas the same phenomenon was not found for the film prepared with GLYMO. It is confirmed that GLYMO is a better precursor than TMSPM for waveguide film preparation. (C) 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved.