Effect of thermal annealing on the optical properties and residual stress of TiO2 films produced by ion-assisted deposition

The effects of thermal annealing of titanium oxide films deposited by ion-beam assistance at annealing temperatures from 100 degrees C to 300 degrees C on the residual stress and optical properties of the films was investigated. The refractive indices and extinction coefficients increased gradually as the temperature was increased from 100 degrees C to 200 degrees C and then declined gradually as the temperature was increased further from 200 degrees C to 300 degrees C. The film lost oxygen and slowly generated lower suboxides as the annealing temperature was reduced below 200 degrees C, as determined by x-ray photoelectron spectroscopy (XPS). As the annealing temperature increased above 200 degrees C, the lower suboxides began to capture oxygen and form stable oxides. XPS measurements were made to verify both the binding energy associated with the Ti 2p line and the variation of the O 1s line. A Twyman-Green interferometer was employed for phase-shift interferometry to study the residual stress. The residual stress declined as the temperature was reduced from 100 degrees C to 200 degrees C because the lower suboxides reduced the stress in the film. Above 200 degrees C, the film began to capture oxygen, so the residual stress rose. At 300 degrees C, the film was no longer amorphous as the anatase was observed by x-ray diffraction.     

Optical properties and residual stress of YbF3 thin films deposited at different temperatures

The influence of deposition temperature on the optical properties, microstructure, and residual stress of YbF(3) films, deposited by electron-beam evaporation, has been investigated. The increased refractive indices and surface roughness of YbF(3) films indicate that the film density and columnar structure size increase with deposition temperature. At the same time, higher packing density reduces absorption of moisture. The residual stress is related to deposition temperature and to substrate. For the samples deposited on BK7, the residual stress mainly comes from intrinsic stress, however, for those on fused silica, thermal stress is the dominant factor of total residual stress.     

退火温度对TiO2薄膜结构与光学性能的影响

研究退火温度对薄膜相结构、表面化学组成、形貌及光学性能的影响.采用射频磁控溅射法在单晶硅片和石英玻璃片上负载TiO2薄膜,通过X射线衍射(XRD)、原子力显微镜(AFM)、X光电子能谱(XPS)和紫外可见光谱(UV-vis)对其进行表征.结果表明,常温制备400℃以下退火的TiO2薄膜为无定形结构,400℃以上退火的TiO2薄膜出现锐钛矿相,600℃以上退火的TiO2薄膜开始出现金红石相,退火温度在1000℃以上时样品已经完全转变为金红石相;高温退火薄膜的组成为TiOx;随着退火温度的升高,薄膜透射率下降,折射率和消光系数有所增加.     

Annealing dependence of residual stress and optical properties of TiO2 thin film deposited by different deposition methods

Titanium oxide (TiO(2)) thin films were prepared by different deposition methods. The methods were E-gun evaporation with ion-assisted deposition (IAD), radio-frequency (RF) ion-beam sputtering, and direct current (DC) magnetron sputtering. Residual stress was released after annealing the films deposited by RF ion-beam or DC magnetron sputtering but not evaporation, and the extinction coefficient varied significantly. The surface roughness of the evaporated films exceeded that of both sputtered films. At the annealing temperature of 300 degrees C, anatase crystallization occurred in evaporated film but not in the RF ion-beam or DC magnetron-sputtered films. TiO(2) films deposited by sputtering were generally more stable during annealing than those deposited by evaporation.     

Structural, morphological and optical properties of thermal annealed TiO thin films

Structural, morphological and optical properties of TiO thin films grown by single source thermal evaporation method were studied. The films were annealed from 300 to 520 °C in air after evaporation. Qualitative film analysis was performed with X-ray diffraction, atomic force microscopy and optical transmittance and reflectance spectra. A correlation was established between the optical properties, surface roughness and growth morphology of the evaporated TiO thin films. The X-ray diffraction spectra indicated the presence of the TiO₂ phase for the annealing temperature above 400 °C.     

Structural and optical properties of BaTi2O5 thin films prepared by pulsed laser deposition at different substrate temperatures

BaTi₂O₅ thin films were prepared on MgO (1 0 0) substrates by pulsed laser deposition. The effect of substrate temperature (T_sub) on the structural and optical properties of the films, such as crystal phase, preferred orientation, crystallinity, surface morphology, optical transmittance and bandgap energy, was investigated. The preferred orientation of the films changed form (7 1 0) to (0 2 0) depending on T_sub, and the b-axis oriented BaTi₂O₅ thin film could be obtained at T_sub = 973–1023 K. The surface morphology of the films was different with changing T_sub, which showed a dense surface with an elongated granular texture at T_sub = 973–1023 K. The crystallinity and surface roughness increased at the elevated substrate temperatures. The as-deposited BaTi₂O₅ thin films were highly transparent with an optical transmittance of ～70%. The bandgap energy was found to decrease with increasing substrate temperature, from 3.76 eV for T_sub = 923 K to 3.56 eV for T_sub = 1023 K.     

Effect of thermal annealing on the optical properties and residual stress of graded-index-like films deposited by radio-frequency ion-beam sputtering

Composite films of Ta-Si oxide and graded-index-like films have been realized by using radio-frequency ion-beam sputtering. The influence of thermal annealing on the optical properties and residual stress of single-layer composite films and graded-index-like films has been studied. The residual stress and optical properties of both types of films were more stable than that of the notch filters fabricated from a series of discrete quarter-wave layers made by alternatively stacking high and low index materials after annealing.     

Influence of thermal annealing on electrical and optical properties of Ga-doped ZnO thin films

Influence of thermal annealing on electrical properties of GZO films has been studied by means of Hall effect measurements and optical characterization based on Drude model analysis for transmission and reflection spectra. Electrical resistivity increased with increasing annealing temperature. Changes of electrical properties were compared between air and N₂ gas atmosphere. Thermal stability in the air was worse compared to the N₂ gas atmosphere. Annealing at rather high temperature caused decrease in the Hall mobility and increase in optical mobility. The difference between the Hall mobility and the optical mobility was attributed to carrier scattering at grain boundaries. Three kinds of deposition method, ion plating using DC arc discharge, DC magnetron sputtering, and RF power superimposed DC magnetron sputtering were compared in terms of the thermal stability.     

Electrical and optical properties of P-doped ZnO thin films by annealing temperatures in Nitrogen ambient

The effects of post-annealing temperature on the optical and electrical properties of P-doped ZnO thin films, grown on sapphire substrate, have been investigated when the annealing is performed under nitrogen ambient. Analysis of the XRD shows that regardless of the post-annealing temperature, the P-doped ZnO thin films have grown the (002) peak. The full width of half maximum decreases from 0.194 to 0.181° as the annealing temperature increases from 700 to 900 °C. This phenomenon means that the increase of annealing temperature causes enhancement of the thin film’s crystalline properties. The results of Hall effect measurements indicate that the P-doped ZnO thin films, annealed at 750 and 800 °C exhibit p-type behavior, with hole concentrations of 5.71 × 10¹⁷ cm⁻³ and 1.20 × 10¹⁸ cm⁻³, and hole mobilities of 0.12 cm²/Vs and 0.08 cm²/Vs, respectively. The low-temperature (10 K) photoluminescence results reveal that the peaks related to the neutral-acceptor exciton (A⁰X) at 3.355 eV, free electrons to neutral acceptor (FA) at 3.305 eV and donor acceptor pair (DAP) at 3.260 and 3.170 eV are observed in the films showing p-type behavior with the acceptors. Because P atoms replace O atoms to produce acceptors from P-doped ZnO thin films by the thermal activation process at the appropriate annealing temperature with nitrogen ambient, the p-type ZnO thin films can be fabricated in this way.     

Influence of thermal annealing on optical properties and surface morphology of NiOx thin films

NiO_x thin films were deposited by reactive DC-magnetron sputtering from a nickel metal target in Ar + O₂ with the relative O₂ content of 5%. Thermal annealing effects on optical properties and surface morphology of NiO_x films were investigated by X-ray photoelectron spectroscopy, thermogravimetric analysis, scanning electron microscope and optical measurement. The results showed that the changes in optical properties and surface morphology depended on the temperature. The surface morphology of the films changed obviously as the annealing temperature increased due to the reaction NiO_x → NiO + O₂ releasing O₂. The surface morphology change was responsible for the variation of the optical properties of the films. The optical contrast between the as-deposited films and 400 °C annealed films was about 52%. In addition, the relationship of the optical energy band gap with the variation of annealing temperature was studied.     

Investigation of optical,structural and morphological properties of nanostructured boron doped TiO 2 thin films

Pure and different ratios (1, 3, 5, 7 and 10%) of boron doped TiO₂ thin films were grown on the glass substrate by using sol–gel dip coating method having some benefits such as basic and easy applicability compared to other thin film production methods. To investigate the effect of boron doped on the physical properties of TiO₂, structural, morphological and optical properties of growth thin films were examined. 1% boron-doping has no effect on optical properties of TiO₂ thin film; however, optical properties vary with > 1%. From X-ray diffraction spectra, it is seen that TiO₂ thin films together with doping of boron were formed along with TiB₂ hexagonal structure having (111) orientation, B₂O₃ cubic structure having (310) orientation, TiB_0·024O ₂ tetragonal structure having rutile phase (110) orientation and polycrystalline structures. From SEM images, it is seen that particles together with doping of boron have homogeneously distributed and held onto surface.     

Structural and electrical properties of RuO2 thin films prepared by rf-magnetron sputtering and annealing at different temperatures

Conductive ruthenium oxide (RuO₂) thin films have been deposited at different substrate temperatures on various substrates by radio-frequency (rf) magnetron sputtering and were later annealed at different temperatures. The thickness of the films ranges from 50 to 700 nm. Films deposited at higher temperatures show larger grain size (about 140 nm) with (200) preferred orientation. Films deposited at lower substrate temperature have smaller grains (about 55 nm) with (110) preferred orientation. The electrical resistivity decreases slightly with increasing film thickness but is more influenced by the deposition and annealing temperature. Maximum resistivity is 861 μΩ cm, observed for films deposited at room temperature on glass substrates. Minimum resistivity is 40 μΩ cm observed for a thin film (50 nm) deposited at 540°C on a quartz substrate. Micro-Raman investigations indicate that strain-free well-crystallized thin films are deposited on oxidized Si substrates.     

Effect of thermal annealing time on optical and structural properties of TeO2 thin films

TeO₂ thin films were deposited on quartz substrates by rf reactive sputtering technique from a Te metal target. The obtained samples were annealed in an argon atmosphere at 450 °C for different annealing times up to 90 min. X-ray diffraction studies revealed that the as-grown samples were amorphous and there was no appreciable change in structure for a short annealing time. Thin films became polycrystalline with the tetragonal (α-phase) structure of tellurium dioxide crystal with the increase of the thermal annealing time. The refractive index and optical energy gap of the films were calculated by modelling transmittance spectra. The optical energy gap decreased continuously from 3.83 eV to 3.71 eV with increasing thermal annealing time.     

Effect of annealing on microstructural and optoelectronic properties of nanocrystalline TiO2 thin films

In this study, semi-transparent nanostructured titanium oxide (TiO₂) thin films have been prepared by sol–gel technique. The titanium isopropoxide was used as a source of TiO₂ and methanol as a solvent and heat treated at 60°C. The as prepared powder was sintered at various temperatures in the range of 400–700°C and has been deposited onto a glass substrate using spin coating technique. The effect of annealing temperature on structural, morphological, electrical and optical properties was studied by using X-ray diffraction (XRD), high resolution transmittance electron microscopy (HRTEM), atomic force microscopy (AFM), scanning electron microscopy (SEM), dc resistivity measurement and optical absorption studies. The XRD measurements confirmed that the films grown by this technique have good crystalline nature with tetragonal-mixed anatase and rutile phases and a homogeneous surface. The HRTEM image of TiO₂ thin film (annealed at 700°C) showed grains of about 50–60?nm in size with aggregation of 10–15?nm crystallites. Electron diffraction pattern shows that the TiO₂ films exhibited a tetragonal structure. SEM images showed that the nanoparticles are fine and varies with annealing temperature. The optical band gap energy decreases with increasing annealing temperature. This means that the optical quality of TiO₂ films is improved by annealing. The dc electrical conductivity lies in the range of 10^?6 to 10^?5?Ω?cm^?1 and it decreases by the order of 10 with increase in annealing temperature from 400°C to 700°C. It is observed that the sample Ti700°C has a smooth and flat texture suitable for different optoelectronic applications.     

Effect of film thickness and annealing on optical properties of TiO2 thin films and electrical characterization of MOS capacitors

Titanium dioxide (TiO₂) thin films were deposited on glass and silicon (100) substrates by the sol–gel method. The influence of film thickness and annealing temperature on optical transmittance/reflectance of TiO₂ films was studied. TiO₂ films were used to fabricate metal–oxide–semiconductor capacitors. The capacitance–voltage (C–V), dissipation–voltage (D–V) and current–voltage (I–V) characteristics were studied at different annealing temperatures and the dielectric constant, current density and resistivity were estimated. The loss tangent (dissipation) increased with increase of annealing temperature.     

基于膜系设计控制薄膜残余应力的研究

残余应力大的薄膜,容易产生脱膜现象,使得薄膜失去所需功能.在激光薄膜领域,残余应力也是薄膜激光损伤阈值难以提高的原因之一.基于热收缩效应模型和弹性力学原理,从薄膜膜系着手提出了控制薄膜残余热应力的膜系设计原则,将该原则的评价函数用于薄膜膜系设计中,采用优化方法可以设计出残余热应力可接受的薄膜.     

Structural and residual stress changes in Mo/a-Si multilayer thin films with annealing

The thermal and mechanical stability of molybdenum and amorphous silicon (Mo/a-Si) optical multilayers (3 and 4 nm nominal thickness of Mo and Si) at 316 °C were studied by annealing experiments. Growth of amorphous Mo-Si interlayers with a stoichiometry of 12 was observed at the Mo/a-Si interfaces. In addition, residual stresses significantly changed in the crystalline Mo and amorphous Si layers with annealing. High resolution electron microscopy, selected area electron diffraction, and X-ray diffraction of the crystalline Mo revealed that tensile stresses increased from 2 to about 10 GPa in the lateral direction (parallel to the interface plane). The compressive strains that developed in the vertical direction (perpendicular to the interface plane) are consistent with Poisson's ratio. Laser deflectometer measurements of thicker (0.1 m) amorphous silicon layers may indicate compressive-stress relaxation in the amorphous silicon with annealing, consistent with other investigations. Overall, the residual stress in a 40-bilayer film changes from about –0.5 to about +1.5 GPa. Structural transformation after relatively short annealing times at the interfaces in the thin amorphous Mo-Si interlayers may rationalize increased tensile strains in the Mo layers.     

Evolutions of residual stress and microstructure in ZrO2 thin films deposited at different temperatures and rates

The residual stress in ZrO₂ thin films prepared by electron beam evaporation was measured by viewing the substrate deformation using an optical interferometer. The influences of deposition temperature and deposition rate on the residual stress have been studied. The results show that residual stress in ZrO₂ thin films varies from tensile to compressive depending on deposition temperature and deposition rate, respectively. The value of compressive stress increases with the increasing of deposition temperature and deposition rate. At the same time, X-ray diffraction measurement was carried out in order to examine the crystallization behavior of the ZrO₂ thin films as a function of deposition temperature and deposition rate. The relationship between the residual stress and the microstructure has also been discussed.     

后处理工艺对BST薄膜残余应力的影响的分析

采用射频磁控溅射在Pt/Ti/SiO2/Si（100）衬底上制备了钛酸锶钡（BST）薄膜，利用气氛炉对薄膜进行晶化处理，晶化后薄膜的应力采用XRD表征。研究其残余应力随退火气氛、退火温度以及退火降温速率变化的趋势，通过对不同后处理工艺参数实验结果的分析，得到较优化的工艺参数，以制备较小残余应力的优质BST薄膜。