Effects of annealing on the optical, structural, and chemical properties of TiO2 and MgF2 thin films prepared by plasma ion-assisted deposition

Effects of thermal annealing at 400 degrees C on the optical, structural, and chemical properties of TiO2 single-layer, MgF2 single-layer, and TiO2/MgF2 narrow-bandpass filters deposited by conventional electron-beam evaporation (CE) and plasma ion-assisted deposition (PIAD) were investigated. In the case of TiO2 films, the results show that the annealing of both CE and PIAD TiO2 films increases the refractive index slightly and the extinction coefficient and surface roughness greatly. Annealing decreases the thickness of CE TiO2 films drastically, whereas it does not vary that of PIAD TiO2 films. For PIAD MgF2 films, annealing increases the refractive index and decreases the extinction coefficient drastically. An x-ray photoelectron spectroscopy analysis suggests that an increase in the refractive index and a decrease in the extinction coefficient for PIAD MgF2 films after annealing may be related to the enhanced concentration of MgO in the annealed PIAD MgF2 films and the changes in the chemical bonding states of Mg 2p, F 1s, and O is. It is found that (TiO2/MgF2) multilayer filters, consisting of PIAD TiO2 and CE MgF2 films, are as deposited without microcracks and are also thermally stable after annealing.     

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.     

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.     

Effects of temperature on columnar microstructure and recrystallization of TiO2 film produced by ion-assisted deposition

Titanium oxide thin films were deposited by electron-beam evaporation with ion-beam-assisted deposition. The effect of the substrate temperature and annealing temperature on the columnar microstructure and recrystallization of titanium oxide was studied. The values of the refractive index varied from 2.26 to 2.4, indicating that the different substrate temperatures affected the film density. X-ray diffraction revealed that all films were amorphous as deposited. At annealing temperatures from 100 degrees C to 300 degrees C, only the anatase phase was formed. As the substrate temperature increased from 150 degrees C to 200 degrees C to 250 degrees C, the recrystallization temperature fell from 300 degrees C through 250 degrees C to 200 degrees C. Changing the substrate temperature resulted in the formation of various types of columnar microstructure, as determined by scanning-electron microscopy. Different columnar structures resulted in different surface morphologies, as measured by atomic-force microscopy.     

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.     

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.     

Effect of thermal annealing on properties of zinc selenide thin films deposited by chemical bath deposition

Zinc selenide films have been deposited on glass substrate by chemical bath deposition method. The resultant films were annealed up to 473 K temperature. The structural properties of zinc selenide thin films have been investigated by X-ray diffraction techniques. The X-ray diffraction spectra showed that zinc selenide thin films are polycrystalline and have a cubic structure. The most preferential orientation is along the (111) direction for all films. The lattice parameter, grain size, and microstrain were calculated and correlated with annealing temperature. The optical properties showed direct band gap values were found to be in the region of 2.69–2.81 eV. The electrical studies shows conductivity increases with increase in annealing temperature. The optoelectric and structural data are discussed from the point of applications based on achieving high performance devices.     

Influence of deposition parameters on the optical and structural properties of TiO2 films produced by reactive d.c. plasmatron sputtering

We investigated the variations in the structure and optical properties of TiO₂ films produced by reactive d.c. plasmatron sputtering with the most important deposition parameters.Over a wide range, the phase composition (ratio of rutile to anatase) and the grain size of the TiO₂ films can be influenced in a controlled manner by variations in the substrate temperature and the oxygen partial pressure.Because of their high refractive index and low light-scattering losses, plasmatron-sputtered TiO₂ films are of great interest in the field of optical interference coatings, e.g. for dielectric multilayer stacks.     

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 the thermal annealing on the electrical and physical properties of SiC thin films produced by RF magnetron sputtering

SiC thin films have been grown by magnetron sputtering process at RF powers in the range of 100 to 400 W followed or not by annealing in inert environment of ultrapure nitrogen at 1000 °C. Physical characterization by Raman and RBS analysis were performed. The Raman spectra have shown corresponding bands of SiC, Si and C for all the samples while RBS characterization showed a higher concentration of Si for higher RF powers. Unannealed and annealed SiC films were used to produce MIS structures. The electrical properties of these structures were analyzed from Capacitance-Voltage (C-V) and Conductance-Voltage (G-V) characteristics. The results showed that the significant leakage current in the accumulation region observed in the unannealed films can be drastically reduced by the annealing process. A model is proposed to account for this leakage process of the MIS structures.     

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.     

Effect of thermal annealing on the properties of a-SiCN:H films by hot wire chemical vapor deposition using hexamethyldisilazane

We investigated the effect of thermal annealing on the properties of a-SiCN:H films prepared by HWCVD using hexamethyldisilazane focusing on the change in the passivation quality. We found that annealing a-SiCN:H films at the temperature around 600 °C led to an effective hydrogen diffusion, resulting in the enhancement of the passivation effect. The performance of cast polycrystalline silicon solar cells using a-SiCN:H films showed a strong dependence on the contact firing temperature. The best efficiency of 13.75% was achieved at the firing temperature of 750 °C.     

热处理对WO3薄膜光学性质的影响

直流反应磁控溅射法制备了WO3薄膜,薄膜在723K纯N2气中被退火处理.热处理前WO3薄膜为无定形态,热处理后为多晶态.采用透射谱和单谐振子模型获得了薄膜的折射率和消光系数,得到退火前后谐振子能量分别为5.77和5.28eV,色散能为19.9和15.9eV.分析表明退火前后吸收边附近均表现出间接带隙的两段线性关系,间接带隙分别为3.14和2.96eV,声子能量为32和149meV,退火后带隙减小推测可能是由于退火薄膜晶化,氧填隙粒子导致的带尾态效应消失的结果.     

Effect of thermal annealing on the structural and mechanical properties of amorphous silicon carbide films prepared by polymer-source chemical vapor deposition

We report on the effect of thermal annealing on the structural and mechanical properties of amorphous SiC thin films prepared by means of a polymer-source chemical vapor deposition process. The chemical bondings of the a-SiC:H films were systematically examined by means of Fourier transform infrared spectroscopy (FTIR). The film composition was measured by X-ray photoelectron spectroscopy, while X-ray reflectivity measurements were used to account for the film density variations caused by the post-annealing treatments over the 750-1200 °C range. In addition, their mechanical properties (hardness and Young's modulus) were investigated by using the nano-indentation technique. FTIR measurements revealed that not only the intensity of a-SiC absorption band linearly increases but also its position is found to shift to a higher wave number as a result of annealing. In addition, the bond density of Si―C is found to increase from (101.6-224.5) × 10²¹ bond·cm^− 3 accompanied by a decrease of Si―H bond density from (2.58-0.46)× 10²¹ bond·cm^− 3 as a result of increasing the annealing temperature (T_a) from 750 to 1200 °C. Annealing-induced film densification is confirmed, as the a-SiC film density is found to increase from 2.36 to ∼ 2.75 g/cm^− 3 when T_a is raised from 750 to 1200 °C. In addition, as T_a is increased from 750 to 1200 °C, both hardness and Young's modulus are found to increase from 15.5 to 17.6 GPa and 155 to 178 GPa, respectively. Our results confirm the previously established linear correlation between the mechanical properties of the a-SiC films and their bond densities.     

Effects of annealing and deposition temperature on the structural and optical properties of AZO thin films

Al-doped ZnO (AZO) thin films were deposited on p- type Si(100) substrate by r.f magnetron sputtering at 200, 300 and 400 °C substrate temperatures. The deposited films were annealed in air atmosphere for 1 h at temperatures of 700, 800 and 900 °C. The deposition temperature and post-deposition annealing effects on structural and optical properties of the AZO samples were analyzed using X-ray diffraction, atomic force microscope and photoluminescence (PL). After annealing, the value of full width half maximum of the diffraction peaks was decreased as well as, the intensity of visible and strong UV PL emission peaks were increased with temperature. However, the deep-level emission related with zinc point defects was removed by annealing of the samples. Results revealed that all of the as-deposited and annealed AZO films have hexagonal structure along (002) direction and their crystallinity were improved with the increased deposition and post-growth annealing temperatures. In addition, the surface roughness and the particle size of the films were increased with increased deposition and annealing temperatures.     

A comparison of TiN films produced by reactive d.c. sputtering and ion-assisted deposition

The properties of TiN films produced by reactive d.c. sputtering have been compared with those formed by deposition during irradiation by 10 keV nitrogen ions. Films were deposited on aluminium, nickel, molybdenum, silicon and titanium substrates which were chosen because they have a range of mechanical properties. The composition of the films has been studied by Rutherford backscattering, nuclear reaction analysis and transmission electron microscopy and data concerning their hardness and adhesion are also presented. It was found that the films produced by ion-assisted deposition (IAD) were nearly stoichiometric TiN with a predominant (100) orientation while the reactively sputtered films were less crystalline and contained a significant amount of oxygen and carbon throughout the film. There was also considerable improvement in the adhesion of the IAD films but their hardness was only marginally improved.     

在Si基底上真空蒸发沉积Ag-MgF2复合薄膜的内应力研究

报道了用电子薄膜应力分布测试仪测量了不同温度、不同厚度的Ag-MgF2复合薄膜的内应力变化情况，得到了基底温度(退火温度)在300～400℃范围内薄膜平均应力最小，且处于张应力向压应力转变区城。XRD分析表明，在Ag-MgF2复合薄膜中Ag对复合薄膜内应力的影响大于MgF2。     

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) ∼500 °C by pulsed laser deposition (PLD) technique and then were annealed at 150-450 °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 °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 °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.