Residual stress of graded-index-like films deposited by radio frequency ion-beam sputtering

In this study, Ta₂O₅-SiO₂ composite films with various proportions of Ta₂O₅ were prepared by radio frequency ion-beam sputtering deposition. The residual stress of each composite film was analyzed. The residual stresses of different graded-index-like layers made of composite films were studied. The results show that the residual stress of a single layered composite film was lower than that of pure SiO₂ or a pure Ta₂O₅ film. Furthermore, when the composite film was made graded-index-like, the residual stress was reduced.     

Investigation of thermal annealing of optical properties and residual stress of ion-beam-assisted TiO2 thin films with different substrate temperatures

Titanium oxide films were prepared by ion-beam-assisted deposition on glass substrates at various substrate temperatures. The effect of the temperature of thermal annealing from 100 degrees C to 300 degrees C on the optical properties and residual stress was investigated. The influence on the stoichiometry and residual stress of titanium oxides deposited at different substrate temperature was discussed. The residual-stress was minimum and the extinction coefficient was maximum at an annealing temperature of 200 degrees C with a substrate temperature of 150 degrees C. However, when the substrate temperature was increased to 200 degrees C and 250 degrees C, the residual stress was minimum and the extinction coefficient was maximum at an annealing temperature of 250 degrees C. The spectra of x-ray photoelectron spectroscopy reveal that the films lost oxygen and slowly generated lower suboxides at the annealing temperature at which the residual stress was minimum and the extinction coefficient was maximum. As the annealing temperature increased above the temperature at minimum stress, the lower suboxides began to capture oxygen and form stable oxides. TiO2 films deposited at substrate temperatures of 200 degrees C and 250 degrees C were more stable than films deposited at 150 degrees C.     

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.     

Influence of thermal annealing and ultraviolet light irradiation on LaF3 thin films at 193 nm

Lanthanum fluoride (LaF3) thin films were prepared by resistive heating evaporation and electron-beam gun evaporation under the same deposition rate, deposition substrate temperature, and vacuum pressure. The coated LaF3 films were then treated by heat annealing and UV light irradiation. The optical properties, microstructures, stress, and laser-induced damage threshold (LIDT) at a wavelength of 193 nm were investigated. The surface roughness, optical loss, stress, and LIDT of the films were improved after the annealing. The films had better properties when irradiated by UV light as compared with heat annealing.     

Characterization of AlF3 thin films at 193 nm by thermal evaporation

Aluminum fluoride (AlF3) was deposited by a resistive heating boat. To obtain a low optical loss and high laser-induced damage threshold (LIDT) at 193 nm, the films were investigated under different substrate temperatures, deposition rates, and annealing after coating. The optical property (the transmittance, refractive index, extinction coefficient, and optical loss) at 193 nm, microstructure (the cross-sectional morphology, surface roughness, and crystalline structure), mechanical property (stress), and LIDT of AlF3 thin films have been studied. AlF3 thin films deposited at a high substrate temperature and low deposition rate showed a lower optical loss. The highest LIDT occurred at the substrate temperature of 150 degrees C. The LIDT of the films prepared at a deposition rate of 2 A/s was higher than that at other deposition rates. The annealing process did not influence the optical properties too much, but it did increase the LIDT and stress.     

Effects of laser irradiation on the structure and optical properties of ZnO thin films

The effects of laser irradiation on the surface microstructure and optical properties of ZnO films deposited on glass substrates were investigated experimentally and compared with those of thermal annealing. X-ray diffraction (XRD) and atomic force microscopy (AFM) measurements showed that the irradiation treatment with an Ar⁺ laser of 514 nm for 5 min improves the crystalline quality of ZnO thin films through increasing the grain size and enhancing the c-axis orientation, with the effects similar to those of the thermal annealing at 500 °C for 1 h. Laser irradiation was found to be more effective both for the relaxation of the residual compressive stress in the as-grown films and for the modification of the surface morphology. A significant increase in the UV absorption and a widening in the optical band-gap of the films were also observed after laser irradiation.     

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.     

Effects of post-deposition annealing on morphology and optical properties of electron beam evaporated Bromoaluminium phthalocyanine thin films

In this paper, effects of post-deposition annealing on morphology and optical properties of electron beam evaporated Bromoaluminium phthalocyanine thin films have been investigated. Surface morphology of the films have been characterized by field emission scanning electron microscopy (FESEM). The FESEM micrographs have shown densely packed nanoparticles and nanorod-like structures for the films annealed at different temperatures. Conditions leading to β-phase have been identified by monitoring post-deposition annealing using optical absorption spectroscopy (UV–Vis). The optical absorption measurements on the as-deposited and annealed films shows that the absorption mechanism is due to direct transition. Also, it is found that the optical band gap decreases with increase in annealing temperature.     

Magnetic anisotropy control in amorphous FeCoSiB films by stress annealing

It is important to control magnetic anisotropy of ferromagnetic materials. In this work, magnetic anisotropy of amorphous FeCoSiB films is controlled by stress annealing. FeCoSiB films are deposited on glass substrate and annealed with stress in vacuum. When the annealed films are released from clamp, permanent tensile or compressive strain can be introduced in the films. Influences of both tensile and compressive strain on the magnetic properties of FeCoSiB films have been studied. The results show that FeCoSiB films by stress annealing exhibit strong magnetic anisotropy while the samples by normal annealing exhibit magnetic isotropy. Easy axis along the stress is induced in the films with tensile stress, while easy axis perpendicular to the stress is induced in the samples with compressive stress. It has also been found that the magnetic anisotropy increases with the increase of the strain. The effects of strain on the magnetic properties of FeCoSiB films have been interpreted by stress induced anisotropy via magnetoelastic coupling.     

Investigation of annealing-treatment on structural and optical properties of sol-gel-derived zinc oxide thin films

The transparent ZnO thin films were prepared on Si(100) substrates by the sol-gel method. The structural and optical properties of ZnO thin films, submitted to an annealing treatment in the 400–700°C ranges are studied by X-ray diffraction (XRD) and UV-visible spectroscopic ellipsometry (SE). XRD measurements show that all the films are crystallized in the hexagonal wurtzite phase and present a random orientation. Three prominent peaks, corresponding to the (100) phase (2θ ≈ 31.8°), (002) phase (2θ ≈ 34.5°), and (110) phase (2θ ≈ 36.3°) appear on the diffractograms. The crystallite size increases with increasing annealing temperature. These modifications influence the optical properties. The optical constants and thickness of the films have been determined by analysing the SE spectra. The optical bandgap has been determined from the extinction coefficient. We found that the refractive index and the extinction coefficient increase with increasing annealing temperature. The optical bandgap energy decreases with increasing annealing temperature. These mean that the optical quality of ZnO films is improved by annealing.     

退火对反应磁控溅射制备ITO薄膜性能影响

采用铟锡合金靶 (铟 锡 ,90 - 10 ) ,通过直流反应磁控溅射在玻璃基片上制备出ITO薄膜 ,并在大气环境下高温退火处理。研究了退火温度对薄膜结构、光学和电学性能的影响。研究表明 ,随着退火温度升高薄膜的电学特性得到很大提高     

Thermal stability of sputtered zirconium oxide films

In this work, the effect of post-growth annealing on the structural and optical properties of sputtered zirconium oxide films has been investigated. The temperature dependence of structure, density, and optical constants has been systematically studied by X-ray diffraction, X-ray reflectometry, atomic force microscopy (AFM) and optical spectroscopy. X-ray diffraction studies show no variation in the crystalline phase upon annealing except grain growth. X-ray reflectivity measurements determine a density increase of approximately 11% and a simultaneous thickness reduction of 10% upon annealing. The surface roughness of the films increases upon annealing as determined by XRR and confirmed by AFM measurements. Optical spectroscopy measurements confirm that the refractive index n of the films decreases with increasing annealing temperature. At the same time the optical band gap E_g of the films increases from 4.58 to 4.97 eV annealing at 900°C. The surprising decrease of refractive index upon annealing is attributed to both the intermixing of Si with ZrO₂ and the increasing surface roughness of the films.     

The effects of annealing temperature on characteristics of UBMS sputtered CNx films for protective coatings

The carbon nitride (CNx) films have been prepared by unbalanced magnetron sputtering (UBMS) at room temperature. The deposited CNx films have been post-annealed at temperatures ranging from 300 °C to 700 °C in increments of 200 °C using rapid thermal annealing (RTA) equipment in vacuum ambient. We investigated the effects of rapid thermal annealing on the structural, surface, and physical properties of CNx films for application of protective coatings. As the result, the increasing annealing temperature led to a decline in physical properties of CNx films such as hardness, elastic modulus, adhesion, frication coefficient, and surface roughness, however it is attributed to the improvement of the residual stress in the film. These results are related to the ordering of sp² bonded clustering and the increase of disordered graphite domain by the desorption of N contents in the films, Specially, high annealing temperature over 700 °C is attributed to the graphitization of film.     

In situ and ex situ investigation on the annealing performance of the ZnO film grown by ion beam deposition

The effects of the post-annealing treatment on the properties of the ZnO thin films deposited by ion beam sputtering have been investigated. By using in situ X-ray diffraction technique, an overview of the crystallization behavior of the ZnO film during the annealing process was obtained. It was found that the whole process can be divided into three regions. The improvement of the film’s crystallinity performance mainly occurs within the annealing temperature ranging from 300 to 600 °C. Both in situ and ex situ XRD results show the shift of the ZnO (002) peak towards high angle with the increasing annealing temperature, which is attributed to the variation of the stress in the film. The stress is mainly caused by the intrinsic stress which is affected by the oxygen deficiency in the film. The oxygen deficiency is sensitive to the annealing ambient. The film annealed in the O₂ ambient has less oxygen deficiency and higher resistivity. All the ZnO films deposited on the glass substrates have an optical transmittance over 85% in the visible region. Our results show that the ZnO films deposited using ion beam sputtering exhibit good thermal stability and high performance after annealing.     

不同退火工艺对AZO膜性能的影响

掺铝氧化锌(AZO)薄膜由于其独特的光学和电学性能而倍受人们的青睐。本文采用射频磁控溅射技术,制备了综合性能优良的AZO薄膜,通过不同退火工艺处理,研究了其对AZO薄膜的组织结构、电学性能及光学性能的影响。氮气环境下的退火使得AZO膜出现了更为明显的蓝移现象,氢气环境下的退火提高了薄膜的导电性。     

TiO2--Ta2O5 composite thin films deposited by radio frequency ion-beam sputtering

TiO2--Ta2O5 composite films were prepared by a radio frequency ion-beam sputtering deposition process, and the refractive indices and extinction coefficients of the composite films were found to be between those of the TiO2 and Ta2O5 films. The structure of the as-deposited films was amorphous, and the surface roughness was approximately 0.1 nm. The residual stress of the composite films was less than that of pure TiO2 film. The structure of the composite films after annealing was amorphous, with low surface roughness and slightly increased residual stress. The film containing 6.3% TiO2 displayed better properties than either the pure TiO2 or the pure Ta2O5 film.     

溶胶—凝胶法制备TiO2—SiO2复合薄膜的研究

采用溶胶－凝胶方法在单晶Ｓｉ基片上制备了ＴｉＯ２－ＳｉＯ２复合薄膜，研究了溶剂、ｐＨ值对先体溶液成胶时间的作用，溶液的浓度、甩胶时的旋转速度、涂覆层数以及热处理温度对薄膜厚度、光学性能的影响。薄膜的折射率随温度增大，其主要贡献来自于薄膜中结构的变化。并测量了薄膜的Ｉ－Ｖ、Ｃ－ｆ特性，由于薄膜中的热击穿效应而使得ＴｉＯ２含量较高的薄膜２的Ｉ－Ｖ呈非线性变化。     

Post annealing effect on structural and optical properties of ZnO thin films derived by sol–gel route

Zinc oxide thin films have been spun coated on p-Si (100) substrates by sol–gel route. These films were annealed at different annealing temperatures from 300 to 1,000 °C in the oxygen ambient. In this way a suitable annealing temperature window for the sol–gel derived ZnO films exhibiting minimum defects (points and dislocations) and better quality (crystal and optical) was investigated. The structural and optical features of ZnO thin films have been examined by X-ray diffraction, atomic force microscopy, UV–Vis spectroscopy, and photoluminescence spectra. The results revealed that the crystallization in the films initiated at 300 °C, improved further with annealing. All the deposited films exhibited wurtzite phase with c-axis orientations. The variations in the position of characteristic (002) peak, stress, strain and lattice parameters are investigated as a function of annealing temperature. The optical band gap is not significantly affected with annealing as observed by UV–Vis transmission spectroscopy. The Photoluminescence spectra exhibited three luminescence centers. The near band edge esmission was observed in UV region which enhanced with the heat treatment, is an indication of improvement in the optical quality of films. The other two visible emissions are related to native defects in ZnO lattice were appeared only for higher annealing (≥700 °C).     

Annealing and partial pressure ratio effects on ZnO films grown by metal-organic chemical vapor deposition using tert-butanol as oxidant

ZnO films were deposited by metal-organic chemical vapor deposition on (0001) sapphire substrates at various partial pressure ratios of oxygen and zinc precursors (R_VI/II). The annealing and the R_VI/II ratio effects on the vibrational and optical properties of ZnO films have been investigated by Micro-Raman scattering and low temperature photoluminescence (PL) spectroscopy. As confirmed by characterizations used in this study, the quality of the ZnO films was improved by thermal annealing at 900 °C in oxygen ambient. Raman spectra of the as-deposited films show a broad band (BB) centered at about 518 cm⁻¹ whose intensity increases when the R_VI/II ratio decreases. After annealing, the intensity ratio of the BB to the E₂ high (E₂^H) peak decreases rapidly with increasing the annealing time (t_an). The vibrational properties of the annealed films grown at R_VI/II = 1 need only 1 h to be improved in contrast to those of films grown in Zn-rich condition, which need 4 h. From the E₂^H mode frequency, the residual stress in both the as-grown and the annealed films has been estimated. Micro-Raman measurements show that as-grown films are under a compressive stress which vanishes upon annealing and is not strongly dependent on t_an for t_an up to 1 h. PL spectra show that sharp donor bound exciton and A-free exciton emissions are observed for the as-deposited films grown at R_VI/II ≥ 0.5 and are enhanced after annealing for 1 h. However, in ZnO films grown in Zn-rich condition these emissions are absent and a t_an = 4 h is needed to annihilate non-radiative recombination centers and improve their luminescent efficiency.     

Diffusion and adhesion properties of Cu films on polyimide substrates

Copper thin films were prepared on polyimide (PI) substrates by physical vapor deposition (PVD) and chemical vapor deposition (CVD). Titanium nitride (TiN) diffusion barrier layers were deposited between the copper films and the PI substrates by PVD. Auger electron spectroscopy compositional depth profile showed that TiN barrier layer was very effective in preventing copper diffusion into PI substrate even after the Cu/TiN/PI samples were annealed at 300 °C for 5 h. For the as-deposited CVD-Cu/PI, CVD-Cu/TiN/PI, and as-deposited PVD-Cu/PI samples, the residual stress in Cu films was very small. Relatively larger residual stress existed in Cu films for PVD-Cu/TiN/PI samples. For PVD-Cu/TiN/PI samples, annealing can increase the peeling strength to the level observed without a diffusion barrier. The adhesion improvement of Cu films by annealing treatment can be attributed to lowering of the residual tensile stress in Cu films.