A Spectroscopic Ellipsometry Study of TiO2 Thin Films Prepared by dc Reactive Magnetron Sputtering： Annealing Temperature Effect

TiO2 thin films are obtained by dc reactive magnetron sputtering. A target of titanium （99.995%） and a mixture of argon and oxygen gases are used to deposit TiO2 films on to silicon wafers （100）. The crystalline structure of deposited and annealed film are deduced by variable-angle spectroscopic ellipsometry （VASE） and supported by x-ray diffractometry. The optical properties of the films are examined by VASE. Measurements of ellipsometry are performed in the spectral range O. 72-3.55 e V at incident angle 75^o. Several SE models, categorized by physical and optical models, are proposed based on the ＇simpler better＇ rule and curve-fits, which are generated and compared to the experimental data using the regression analysis. It has been found that the triple-layer physical model together with the Cody-Lorentz dispersion model offer the most convincing result. The as-deposited films are found to be inhomogeneous and amorphous, whereas the annealed films present the phase transition to anatase and rutile structures. The refractive index of TiO2 thin films increases with annealing temperature. A more detailed analysis further reveals that thickness of the top sub-layer increases, whereas the region of the bottom amorphous sub-layer shrinks when the films are annealed at 300℃.     

Optical Characterization of rf-Magnetron Sputtered Nanostructured SnO2 Thin Films

Tin oxide （Sn02 ） thin films are deposited by rf-magnetron sputtering and annealed at various temperatures in the range of 100-500 ℃ for 15 min. Raman spectra of the annealed films depict the formation of a small amount of SnO phase in the tetragonal Sn02 matrix, which is verified by x-ray diffraction. The average particle size is found to be about 20-30 nm, as calculated from x-ray peak broadening and SEM images. Various optical parameters such as optical band gap energy, refractive index, optical conductivity, carrier mobility, carrier concentration etc. are determined from the optical transmittance and reflectance data recorded in the wavelength range 250-2500 nm. The results are analyzed and compared with the data in the literature.     

Laser Induced Damage Threshold at 355 and 1064nm of Ta2O5 Films of Different Phases

Ta2O5 films axe deposited on fused silica substrates by conventional electron beam evaporation method. By annealing at different temperatures, Ta2 O5 films of amorphous, hexagonal and orthorhombic phases are obtained and confirmed by x-ray diffractometer （XRD） results. X-ray photoelectron spectroscopy （XPS） analysis shows that chemical composition of all the films is stoichiometry. It is found that the amorphous Ta2 O5 film achieves the highest laser induced damage threshold （LIDT） either at 355 or 1064nm, followed by hexagonal phase and finally orthorhombic phase. The damage morphologies at 355 and 1064nm are different as the former shows a uniform fused area while the latter is centred on one or more defect points, which is induced by different damage mechanisms. The decrease of the LIDT at 1064nm is attributed to the increasing structural defect, while at 355nm is due to the combination effect of the increasing structural defect and decreasing band gap energy.     

Multilayer Au/TiO2Composite Films with Ultrafast Third-Order Nonlinear Optical Properties

We report on the ultrafast third-order optical nonlinearity in multilayer Au/TiO2 composite films fabricated on quartz substrates by pulsed laser deposition technique. The linear optical properties of the films are determined and optical absorption peaks due to surface plasmon resonance of Au particles are observed at about 590hm. The third-order optical nonlinearities of the films are investigated by z-scan method using a femtosecond laser （50 fs） at the wavelength of 800 nm. The sample showed fast nonlinear optical responses with nonlinear absorption coefficient and nonlinear refractive index being -3.66 × 10^-10 m/W and -2.95 × 10^-17 m^2/W, respectively. The results also show that the nonlinear optical effects increase with the increasing Au concentration in the composite films.     

Influence of Different Substrates on Laser Induced Damage Thresholds at 1064nm of Ta2O5 Films

Ta2O5 films are prepared on Si, BK7, fused silica, antireflection （AR） and high reflector （HR） substrates by electron beam evaporation method, respectively. Both the optical property and laser induced damage thresholds （LIDTs） at 1064 nm of Ta2O5 films on different substrates are investigated before and after annealing at 673 K for 12 h. It is shown that annealing increases the refractive index and decreases the extinction index, and improves the O/Ta ratio of the Ta2O5 films from 2.42 to 2.50. Moreover, the results show that the LIDTs of the Ta2O5 films are mainly correlated with three parameters： substrate property, substoichiometry defect in the films and impurity defect at the interface between the substrate and the films. Details of the laser induced damage models in different cases are discussed.     

Effects of Annealing on Microstructure and Optical Properties of TiO2 Sculptured Thin Films

The evolution of microstructure and optical properties of TiO2 sculptured thin films under thermal annealing is reported. XRD, field emission SEM, UV-Vis-NIR spectra are employed to characterize the microstructural and optical properties. It is found that the optimum annealing temperature for linear birefringence is 500℃. The maximum of transmission difference for linear birefringence is up to 18%, which is more than twice of that in as-deposited thin films. In addition, the sample annealed at 500℃ has a minimum of column angle about 12℃. The competitive process between the microstructural and optical properties is discussed in detail. Post-annealing is a useful method to improve the linear birefringence in sculptured thin films for practical applications.     

Comparison of TiO2 and ZrO2 Films Deposited by Electron-Beam Evaporation and by Sol-Gel Process

TiO2 and ZrO2 films are deposited by electron-beam （EB） evaporation and by sol-gel process. The film properties are characterized by visible and Fourier-transform infrared spectrometry, x-ray diffraction analysis, surface roughness measure, absorption and laser-induced damage threshold （LIDT） test. It is found that the sol-gel films have lower refractive index, packing density and roughness than EB deposited films due to their amorphous structure and high OH group concentration in the film. The high LIDT of sol-gel films is mainly due to their amorphous and porous structure, and low absorption. LIDT of EB deposited film is considerably affected by defects in the film, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.     

Structure and optical properties of ZnS thin films grown by glancing angle deposition

The glancing angle deposition (GLAD) technique was used to deposit ZnS films by electron beam evaporation method. The cross sectional scanning electron microscopy (SEM) image illustrated a highly orientated microstructure composed of slanted column. The atomic force microscopy (AFM) analysis indicated that incident flux angle had significant effects on the nodule size and surface roughness. Under identical nominal thickness, the actual thickness of the GLAD films is related to the incident flux angle. The refractive index and in-plane birefringence of the GLAD ZnS films were discussed, and the maximum birefringence Δn = 0.036 was obtained at incident flux angle of α = 80°. Therefore, the glancing angle deposition technique is a promising way to create a columnar structure with enhanced birefringent property.     

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.     

Effects of Annealing Temperature on Structural and Optical Properties of ZnO Thin Films

The effects of annealing temperature on the structural and optical properties of ZnO films grown on Si （100） substrates by sol-gel spin-coating are investigated. The structural and optical properties are characterized by x-ray diffraction, scanning electron microscopy and photoluminescence spectra. X-ray diffraction analysis shows the crystal quality of ZnO films becomes better after annealing at high temperature. The grain size increases with the temperature increasing. It is found that the tensile stress in the plane of ZnO films first increases and then decreases with the annealing temperature increasing, reaching the maximum value of 1.8 GPa at 700℃. PL spectra of ZnO films annealed at various temperatures consists of a near band edge emission around 380 nm and visible emissions due to the electronic defects, which are related to deep level emissions, such as oxide antisite （OZn）, interstitial oxygen （Oi）, interstitial zinc （Zni） and zinc vacancy （VZn^-）, which are generated during annealing process. The evolution of defects is analyzed by PL spectra based on the energy of the electronic transitions.     

Chemical Oxidation of La2CuO4 Epitaxial Thin Films Grown by Pulsed Laser Deposition

Chemical oxidation is used to induce superconductivity in La2CuO4 expitaxial thin films fabricated by pulsed laser deposition technique. Details about the influence of oxidation time on structural, surface morphology, Raman spectra, and electrical properties have been investigated. The results convince that successful uptake of oxygen occurs in the oxidized films, and the content of the inserted oxygen increases with increasing oxidation interval. The possible mechanism for the excess oxygen insertion into the film is also discussed.     

Influence of substrate temperature on properties of MgF2 coatings

Thermal boat evaporation was employed to prepare MgF₂ single-layer coatings upon both JGS1 and UBK7 substrates at different substrate temperatures. Microstructure, transmittance and residual stress of these coatings were measured by X-ray diffraction, spectrophotometer, and optical interferometer, respectively. Measurement of laser induced damage threshold (LIDT) of the samples was performed at 355 nm, 8 ns pulses. The results showed that high substrate temperature was beneficial to crystallization of the film. Above 244 °C, the refractive index increased gradually with the substrate temperature rising. Whereas, it was exceptional at 210 °C that the refractive index was higher than those deposited at 244 and 277 °C. The tensile residual stresses were exhibited in all MgF₂ films, but not well correlated with the substrate temperature. In addition, the stresses were comparatively smaller upon JGS1 substrates. A tendency could be seen that the LIDTs reached the highest values at about 244 °C, and the films upon JGS1 had higher LIDTs than those upon UBK7 substrates at the same temperature. Meanwhile, the damage morphologies showed that the laser damage of the coating resulted from an absorbing center at the film-substrate interface. The features of the damages were displayed by an absorbing center dominated model. Furthermore, the reason of the difference in LIDT values was discussed in detail.     

Determination of Thickness and Optical Constants of ZnO Thin Films Prepared by Filtered Cathode Vacuum Arc Deposition

ZnO thin films are prepared on glass substrates by filtered cathode vacuum arc （FCVA） deposition technique. A new method is demonstrated to extract the refractive index, thickness and optical band gap of ZnO thin films from the transmission spectrum alone. The refractive index is calculated from the extremes of the interference fingers. The transmission spectrum is divided into two terms, non-interference term and interference effect term. The thickness of thin films is calculated by simulating the interference term, and the non-interference term is used to calculate optical band gap with the gained thickness. The results are compared with measurements by using an ellipsometry and a scanning electron microscope.     

Microstructure of Epitaxial Er2O3 Thin Film on Oxidized Si (111) Substrate

Er₂O₃ thin films are grown on oxidized Si (111) substrates by molecular beam epitaxy. The sample grown under optimized condition is characterized in its microstructure, surface morphology and thickness using grazing incidence x-ray diffraction (GIXRD), atomic force morphology and x-ray reflectivity. GIXRD measurements reveal that the Er₂O₃ thin film is a mosaic of single-crystaldomains. The interplanar spacing d in-plane residual strain tensor ε_| and the strain relaxation degree ξ are calculated. The Poisson ratio μ obtained by conventional x-ray diffraction is in good agreement with that of the bulkEr₂O₃. In-plane strains in three sets of planes, i.e. (440), (404), and (044), are isotropic.     

Synthesis of LECBD grown cluster assembled SeO2 thin films

Cluster assembled selenium oxide (SeO₂) thin films, as a function of oxygen flow pressure (OFP) have been synthesized by a low energy cluster beam deposition (LECBD) technique. The OFP dependent surface morphology leading to well separated nanoclusters (size ranging from 50 to 200 nm) and fractal features are confirmed from transmission electron microscopic (TEM) measurements. A diffusion limited aggregation (DLA) mediated fractal growth with dimension as 1.71 ± 0.01 has been observed for high OFP (60 mbar). Structural analysis by glancing angle X-ray diffraction (GXRD) and selected area diffraction (SAD) studies identify the presence of tetragonal phase SeO₂ in the deposit. Micro-Raman studies indicate the shifts in bending and stretching vibrational phonon modes in cluster assembled SeO₂ as compared to their bulk counter part due to the phonon confinement effect.     

Laser Molecular Beam Epitaxy of Multilayer Heterostructure SrNb0.05Ti0.95O3/La0.9Sr0.1MnO3 in 10000 Unit-Cell Layers

Ten thousands of unit-cell multilayer heterosturctures, [SrNb0.05 Ti0.95O3/La0.9 Sr0.1MnO3]3 （SNTO/LSMO）, have been epitaxial grown on SrTiO3 （001） substrates by laser molecular beam epitaxy. The monitor of insitu. reflection high-energy electron diffraction demonstrates that the heterosturctures are layer-by-layer epitaxial growth. Atomic force microscope observation indicates that the surface of the heterosturcture is atomically smooth. The measurements of cross-sectional low magnification and high-resolution transmission electron microscopy as well as the corresponding selected area electron diffraction reveal that the interfaces are of perfect orientation, and the epitaxial crystalline structure shows the orientation relation of SNTO（001）//LSMO（001）, and SNTO[100]//LSMO[100].     

Electroluminescence from Multilayered Diamond/CeF3/SiO2 Films

We report a thin film electroluminescent device with a three-layer structure （diamond/CeF3/SiO2 films）, which has a luminance of 1.5 cd/m^2 at dc voltage 215 V. The electroluminescence spectrum at room temperature shows that the main peaks locate at 527 and 593nm, which are attributed to isolated emission centers of Ce^3＋ ions.     

Microstructures and electrical properties of La0.8Sr0.2MnO3 films synthesized by sol-gel method

La_0.8Sr_0.2MnO₃ (LSMO) thin films were fabricated on alumina substrates by an improved sol-gel dip-coating process. It was found that multiple dip-coating process could not be performed until the pre-firing temperature reached 600 °C. Different amounts of LSMO powders were added to precursor solution with an aim to avoid cracks in LSMO thin films during calcining caused by the shrinkage mismatch between the film and the substrate. The structure and surface morphology of the films prepared from precursors with and without LSMO powders were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). It was found that the addition of 56.4 wt.% LSMO powders into the sol-gel precursor solution significantly modified the microstructure of films. A single LSMO perovskite phase was obtained on alumina substrate after calcining at 800 °C for 4 h by the improved sol-gel method. The sheet resistance of the films prepared with different processing parameters was measured by four-point dc method. Results indicated that the sheet resistance of films decreased with increasing the number of coating applications and the amount of LSMO powders.     

Ferroelectric Properties of Bi3.25La0.75Ti3O12 Thin Films Crystallized inDifferent N2/O2 Ambients

Bi3.25La0.75 Ti3O12 （BLT） ferroelectric thin films are deposited by sol-gel method and annealed for crystallizaion in total l eccm N2/02 mixed gas with various ratio at 750℃ for 30rain. The effect of crystallization ambient on the structural and ferroelectric properties of the BLT films is studied. The growth direction and grain size of BLT film are revealed to affect ferroeleetric properties. Alter the BLT film is annealed in 20%O2, the largest P~ value is obtained, which is ascribed to an increase of random orientation and large grain size. The fatigue property is improved with the concentration of oxygen in the ambient increasing, which is ascribed to annealing in the ambient with high concentrated oxygen adequately decreasing the defects related to lack of oxygen.     

Annealing Induced Aggregations and Sign Alterations of Nonlinear Absorption and Refraction of Dense Au Nanoparticles in TiO2 Films

Au-TiO2 dis-conductive composite films with Au atom concentrate as high as 82% are prepared by using reactive co-sputtering technique. The annealing effect on the nanostructures and optical nonlinearities of the composite films are investigated. A u nanoparticles aggregated to semi-continuum network structures during the annealing processes. As the annealing temperature increases from 25℃ to 400℃, the surface plasmon absorption band is shifted and its strength is increased, consequently, the nonlinear absorption coefficient β decreases from 5.6 × 10^4 cm/GW to -1.7 × 10^4 cm/GW, while the nonlinear refractive index ~ increases from -0.95 cm^2/GW to 1.3 cm^2/GW.