射频磁控溅射法制备TiO2-xNX薄膜的结构性能研究

利用射频磁控溅射法室温下在Si（100）衬底上制备了N掺杂的TiO2薄膜，并且采用x射线衍射（XRD）、X射线光电子能谱（XPS）和透射光谱对薄膜进行了表征。XRD结果表明在纯Ar和N2（33．3％）／Ar气氛下制备的TiO2-xNx薄膜均为单一的金红石相，薄膜结晶性良好，呈高度（211）择优取向，而在N2（50．0％）／Ar下制备的薄膜结晶性明显变差；对于N掺杂的TiO2薄膜，XPS表明部分N原子进入TiO2晶格，并且以N—Ti—O、N—O键以及间隙式N原子形式存在；透射光谱表明掺N后的TiO2薄膜吸收边发生了红移。

Investigation on microstructure and optical properties of titanium dioxide coatings annealed at various temperature

TiO2 coatings were prepared on fused silica with conventional electron beam evaporation deposition. After TiO2 thin films were annealed at different temperatures for 4 h, several properties were investigated by X-ray diffraction (XRD), spectrometer.. photoelectron spectroscopy (XPS) and AFM. It was found that with the annealing temperature increasing, the transmittance of TiO2 coatings decreased, and the cutoff wavelength shifted to long wavelength in near ultraviolet band. Especially, when coatings were annealed at high temperature, the optical loss is very serious, which can be attributed to the scattering and the absorption of TiO2 coatings. XRD patterns revealed that only anatase phase was observed in TiO2 coatings regardless of the different annealing temperatures. XPS results indicated that the fine chemical shift of TiO2 2p(1/2) should be attributed to existence of oxygen vacancies around Ti+4 ion. The investigation on surface morphology by AFM showed that the RMS of titania thin films gradually increases from less than 0.40 nm to 5.03 nm and it should be ascribed to the growth of titanium dioxide grain size with the increase of annealing temperature. (C) 2005 Elsevier B.V. All rights reserved.

TiO2添加剂对镁钙质耐火材料防水化性能的影响

通过对TiO2添加剂的理论分析和基质的水化试验，研究了TiO2对镁钙耐火材料防水化性能的影响．结果表明：理论分析和实验结果相符合，TiO2添加剂的加入有效抑制了镁钙耐火材料的水化，TiO2添加剂的加入量以3％最佳。

真空中有机污染物对TiO2/SiO2介质膜损伤阈值的影响

本文主要研究了真空中有机污染物对薄膜阈值的影响。采用电子枪蒸镀的方式制备了由TiO2/SiO2两种材料组合而成的1064nm高反膜，分别在大气和真空中对其损伤阈值进行了测量。发现在真空中污染物易黏附于光学元件表面，导致损伤；真空中的氧分子会加速损伤过程，根据破斑形貌的分析认为是由于在激光作用下氧分子与有机污染物发生反应造成的；真空中的有机污染物被去除后，真空和大气中的损伤阈值差别不大，破斑形貌相似。结果表明有机污染物是真空中损伤阈值降低的主要原因。

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 Elms 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 Elm, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.

Effect of process parameters on laser damage threshold of TiO2 coatings

We investigate the laser damage behaviour of an electron-beam-deposited TiO2 monolayer at different process parameters. The optical properties, chemical composition, surface defects, absorption and laser-induced damage threshold (LIDT) of Elms are measured. It is found that TiO2 Elms with the minimum absorption and the highest LIDT can be fabricated using a TiO2 starting material after annealing. LIDT is mainly related to absorption and is influenced by the non-stoichiometric defects for TiO2 films. Surface defects show no evident effects on LIDT in this experiment.

Influence of annealing temperature on structure, optical loss and laser-induced damage threshold of TiO2 thin films

TiO2 thin films are prepared on fused silica with conventional electron beam evaporation deposition. After annealed at different temperatures for 4h, the spectra and XRD patterns of the TiO2 thin film are obtained. Weak absorption of coatings is measured by the surface thermal lensing technique, and laser-induced damage threshold (LIDT) is determined. It is found that with the increasing annealing temperature, the transmittance of TiO2 films decreases. Especially when coatings are annealed at high temperature over 1173K, the optical loss is very serious. Weak absorption detection indicates that the absorption of coatings decreases firstly and then increases, and the absorption and defects play major roles in the LIDT of TiO2 thin films.

Structural and optical properties of nanostructured TiO2 thin films fabricated by glancing angle deposition

TiO2 films deposited by electron beam evaporation with glancing angle deposition (GLAD) technique were reported. The influence of flux angle on the surface morphology and the microstructure was investigated by scanning electron microscopy. The GLAD TiO2 films are anisotropy with highly orientated nanostructure of the slanted columns. With the increase of flux angle, refractive index and packing density decrease. This is caused by the shadowing effect dominating film growth. The anisotropic structure of TiO2 films results in optical birefringence, which reaches its maximum at the flux angle alpha = 65 degrees. The maximum birefringence of GLAD TiO2 films is higher than that of common bulk materials. It is suggested that glancing angle deposition may offer an effective method to obtain tailorable refractive index and birefringence in a large continuous range. (c) 2006 Elsevier B.V. All rights reserved.

Effects of oxygen partial pressure on packing density and laser damage threshold of TiO2 thin films

TiO2 films are deposited by electron beam evaporation as a function of oxygen partial pressure. The packing density, refractive index, and extinction coefficient all decrease with the increase of pressure, which also induces the change of the film's microstructure, such as the increase of voids and H2O concentration in the film. The laser-induced damage threshold (LIDT) of the film increases monotonically with the rise of pressure in this experiment. The porous structure and low nonstoichiometric defects absorption contribute to the film's high LIDT. The films prepared at the lowest and the highest pressure show nonstoichiometric and surface-defects-induced damage features, respectively.(C) 2007 American Institute of Physics.

Effects of annealing on laser-induced damage threshold of TiO2/SiO2 high reflectors

The mechanism of improving 1064 nm, 12 ns laser-induced damage threshold (LIDT) of TiO2/SiO2 high reflectors (HR) prepared by electronic beam evaporation from 5.1 to 13.1 J/cm(2) by thermal annealing is discussed. Through optical properties, structure and chemical composition analysis, it is found that the reduced atomic non-stoichiometric defects are the main reason of absorption decrease and LIDT rise after annealing. A remarkable increase of LIDT is found at 300 degrees C annealing. The refractive index and film inhomogeneity rise, physical thickness decrease, and film stress changes from compress stress to tensile stress due to the structure change during annealing. (c) 2007 Elsevier B.V. All rights reserved.

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 degrees C. 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 degrees C has a minimum of column angle about 12 degrees C. 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.

Investigation on properties of TiO2 thin films deposited at different oxygen pressures

TiO2 thin films were prepared by electron beam evaporation at different oxygen partial pressures. The influences of oxygen partial pressure on optical, mechanical and structural properties of TiO2 thin films were studied. The results showed that with the increase of oxygen partial pressure, the optical transmittance gradually increased, the transmittance edge gradually shifted to short wavelength, and the corresponding refractive index decreased. The residual stresses of all samples were tensile, and the value increased as oxygen partial pressure increasing, which corresponded to the evolutions of the packing densities. The structures of TiO2 thin films all were amorphous because deposition particles did not possess enough energy to crystallize. (C) 2007 Elsevier Ltd. All rights reserved.

Investigation on thermal stability of TiO2 films for application at high temperature

The thermal stability of electron beam deposited TiO2 monolayers and TiO2/SiO2 high reflectors (HR) during 300 to 1100 degrees C annealing is studied. It is found that the optical loss of film increases with the increase in annealing temperature, due to the phase change, crystallisation and deoxidising of film. Scattering loss dominates the optical property degradation of film below 900 degrees C, while the absorption is another factor at 1100 degrees C. The increase in refractive index and decrease in physical thickness of TiO2 layer shift the spectra of HR above 900 degrees C. The possible crack mechanism on the surface of HR during annealing is discussed. Guidance for application on high temperature stable optical coatings is given.

High refractive index TiO2 film deposited by electron beam evaporation

The well known 'crystal seed' theory is first applied in this work to prepare TiO2 film: a high refractive index rutile TiO2 film is grown by electron beam evaporation on the rutile seed formed by 1100 degrees C annealing. The average n is larger than 2.4, by far the highest in all the authors' TiO2 films. The films are characterised by optical properties, microstructure and surface morphologies. It is found that the refractive index shows positive relation with the crystal structure, grain size, and packing density and roughness of the film. The film has lower density of granularity and nodule defects on the surface than those of the film deposited by magnetron sputtering. The result shows attractive application in complex filter and laser coatings.