Annealing effects on electron-beam evaporated Al2O3 films

The effects of post-deposited annealing on structure and optical properties of electron-beam evaporated Al2O3 single layers were investigated. The films were annealed in air for 1.5 h at different temperatures from 250 to 400 degrees C. The optical constants and cut-off wavelength were deduced. Microstructure of the samples was characterized by X-ray diffraction (XRD). Profile and surface roughness measurement instrument was used to determine the rms surface roughness. It was found that the cut-off wavelength shifted to short wavelength as the annealing temperature increased and the total optical loss decreased. The film structure remained amorphous even after annealing at 400 degrees C temperature and the samples annealed at higher temperature had the higher rms surface roughness. The decreasing total optical loss with annealing temperature was attributed to the reduction of absorption owing to oxidation of the film by annealing. Guidance to reduce the optical loss of excimer laser mirrors was given. (c) 2004 Elsevier B.V. All rights reserved.

温梯法蓝宝石（Al2O3）晶体的脱碳去色退火研究

温度梯度法（TGT）生长的Al2O3晶体因石墨发热体在高温时的挥发和原料中过渡性金属离子的存在，晶体在不同部位呈现不同颜色，一般上部为浅红色，尾部为浅黄绿色，将TGT法生长的Al2O3晶体（Ф110×80mm^3）依次经过高温氧化气氛、高温还原气氛脱碳、去色退火实验，即“两步法”退火实验，晶体变成无色、透明，经测试，Al2O3晶体的完整性、光学透过率和光学均匀性均有显著提高。

Annealing effects on the optical and structural properties of Al2O3/SiO2 films as UV antireflection coatings on 4H-SiC substrates

Al2O3/SiO2 films have been prepared by electron-beam evaporation as ultraviolet (UV) antireflection coatings on 4H-SiC substrates and annealed at different temperatures. The films were characterized by reflection spectra, ellipsometer system, atomic force microscopy (AFM), X-ray diffraction (XRD) and Xray photoelectron spectroscopy (XPS), respectively. As the annealing temperature increased, the minimum reflectance of the films moved to the shorter wavelength for the variation of refractive indices and the reduction of film thicknesses. The surface grains appeared to get larger in size and the root mean square (RMS) roughness of the annealed films increased with the annealing temperature but was less than that of the as-deposited. The Al2O3/SiO2 films maintained amorphous in microstructure with the increase of the temperature. Meanwhile, the transition and diffusion in film component were found in XPS measurement. These results provided the important references for Al2O3/SiO2 films annealed at reasonable temperatures and prepared as fine anti-reflection coatings on 4H-SiC-based UV optoelectronic devices. (c) 2008 Elsevier B.V. All rights reserved.

Al2O3 Obtained through resistive evaporation for use as insulating layer in transparent field effect transistor

Alumina thin films have been obtained by resistive evaporation of Al layer, followed by thermal oxidation achieved by annealing in appropriate atmosphere (air or O2-rich), with variation of annealing time and temperature. Optical and structural properties of the investigated films reveal that the temperature of 550°C is responsible for fair oxidation. Results of surface electrical resistivity, Raman and infrared spectroscopies are in good agreement with this finding. X-ray and Raman data also suggest the crystallization of Si nuclei at glass substrate-alumina interface, which would come from the soda-lime glass used as substrate. The main goal in this work is the deposition of alumina on top of SnO2 to build a transparent field-effect transistor. Some microscopy results of the assembled SnO2/Al2O3 heterostructure are also shown.

Crack formation due to annealing of Al2O3 films grown on Si(100) by MOCVD

We report crack formation in alumina films grown on Si(100), caused by annealing in a controlled oxidizing ambient. The films were grown in a low-pressure CVD reactor, using aluminium acetylacetonate as precursor. High purity argon and nitrous oxide were employed as carrier and oxidizing gas, respectively. The films were characterized by optical microscopy and SEM/EDAX. The proportion and chemical nature of the heteroatoms, namely C and H, incorporated into the films from the precursor, were characterized by XPS, and FTIR. As-deposited films do not exhibit any cracks, while post-deposition annealing results in cracks. Apart from the delamination of the films, annealing in nitrous oxide ambient leads to an unusual crack geometry, which we term the “railway-track”. These twin cracks are very straight and run parallel to each other for as much as several millimeters. Often, two such linear tracks meet at exactly 90°. Between some of these tracks lie bullet-like structures with very sharp tips, oriented in a specific direction. As cracks are generally activated by residual stress, both thermal and intrinsic, the origins of the stresses that generate these linear cracks are discussed. The redistribution of stress, arising from the removal of C and H during annealing, will also be discussed. An attempt has been made to correlate the formation of cracks with the crystal structure of the film.

Effect of Post-Deposition Annealing on the Al2O3/Si(100) Interface Properties

In the present investigation, Al2O3 thin films were deposited onto Si < 100 > substrates by DC reactive magnetron sputtering. The films were annealed in vacuum for one hour at 623, 823 and 1023 K. The composition of the films was quantitatively estimated using X-ray photoelectron spectroscopy (XPS) and the O/Al ratio was found be in the range 1.19 to 1.43. Grazing incidence X-ray diffraction (GIXRD) results revealed that the annealed films are amorphous in nature. Cross sectional transmission electron microscopy (X-TEM) analysis was carried out to study the microstructure and nature of the Al2O3-Si interface as a function of post-deposition annealing. TEM results revealed the presence of nanocrystalline gamma-Al2O3 in the annealed films and an amorphous interface layer was observed at the Al2O3 Si interface. The thickness of the amorphous interface layer was determined from the TEM analysis and the results are discussed.

Effect of post-deposition annealing on composition and electrical properties of dc reactive magnetron sputtered Al2O3 thin films

We have investigated the effect of post- deposition annealing on the composition and electrical properties of alumina (Al2O3) thin films. Al2O3 were deposited on n-type Si < 100 >. substrates by dc reactive magnetron sputtering. The films were subjected to post- deposition annealing at 623, 823 and 1023 K in vacuum. X-ray photoelectron spectroscopy results revealed that the composition improved with post- deposition annealing, and the film annealed at 1023 K became stoichiometric with an O/Al atomic ratio of 1.49. Al/Al2O3/Si metal-oxide-semiconductor (MOS) structures were then fabricated, and a correlation between the dielectric constant epsilon(r) and interface charge density Q(i) with annealing conditions were studied. The dielectric constant of the Al2O3 thin films increased to 9.8 with post- deposition annealing matching the bulk value, whereas the oxide charge density decreased to 3.11 x 10(11) cm(-2.) Studies on current-voltage IV characteristics indicated ohmic and Schottky type of conduction at lower electric fields (<0.16 MV cm(-1)) and space charge limited conduction at higher electric fields.

Heteroepitaxial growth and annealing of gamma-Al2O3 thin films on silicon

The gamma-Al2O3 films were grown on Si (100) substrates using the sources of TMA (Al (CH3)(3)) and O-2 by very low-pressure chemical vapor deposition (VLP-CVD). It has been found that the gamma-Al2O3 film has a mirror-like surface and the RMS was about 2.5nm. And the orientation relationship was gamma-Al2O3(100)/Si(100). The thickness uniformity of gamma-Al2O3 films for 2-inch epi-wafer was less than 5%. The X-ray diffraction (XRD) and reflection high-energy electron diffraction (RHEED) results show that the crystalline quality of the film was improved after the film was annealed at 1000degreesC in O-2 atmosphere. The high-frequency C-V and leakage current of Al/gamma-Al2O3/Si capacitor were also measured to verify the annealing effect of the film. The results show that the dielectric constant increased from 4 to 7 and the breakdown voltage for 65-nm-thick gamma-Al2O3 film on silicon increases from 17V to 53V.

Heteroepitaxial growth and annealing of gamma-Al2O3 thin films on silicon

The gamma-Al2O3 films were grown on Si (100) substrates using the sources of TMA (Al (CH3)(3)) and O-2 by very low-pressure chemical vapor deposition (VLP-CVD). It has been found that the gamma-Al2O3 film has a mirror-like surface and the RMS was about 2.5nm. And the orientation relationship was gamma-Al2O3(100)/Si(100). The thickness uniformity of gamma-Al2O3 films for 2-inch epi-wafer was less than 5%. The X-ray diffraction (XRD) and reflection high-energy electron diffraction (RHEED) results show that the crystalline quality of the film was improved after the film was annealed at 1000degreesC in O-2 atmosphere. The high-frequency C-V and leakage current of Al/gamma-Al2O3/Si capacitor were also measured to verify the annealing effect of the film. The results show that the dielectric constant increased from 4 to 7 and the breakdown voltage for 65-nm-thick gamma-Al2O3 film on silicon increases from 17V to 53V.

Properties of Al2O3 films prepared by argon ion assisted deposition

Aluminum oxide films have been prepared by ion assisted deposition using argon ions with energy in the range 300 to 1000 eV and current density in the range 50 to 220 μA/cm2. The influence of ion energy and current density on the optical and structural properties has been investigated. The refractive index, packing density, and extinction coefficient are found to be very sensitive to the ion beam parameters and substrate temperatures. The as-deposited films were found to be amorphous and could be transformed into crystalline phase on annealing. However, the crystalline phases were different in films prepared at ambient and elevated substrate temperatures.

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al2O3) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 degrees C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al2O3-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance. AC conductivity and activation energy were determined and the results are discussed. (C) 2011 Elsevier B.V. All rights reserved.

Composition, structure and electrical properties of DC reactive magnetron sputtered Al2O3 thin films

Thin films of alumina (Al2O3) were deposited over Si < 1 0 0 > substrates at room temperature at an oxygen gas pressure of 0.03 Pa and sputtering power of 60 W using DC reactive magnetron sputtering. The composition of the as-deposited film was analyzed by X-ray photoelectron spectroscopy and the O/Al atomic ratio was found to be 1.72. The films were then annealed in vacuum to 350, 550 and 750 degrees C and X-ray diffraction results revealed that both as-deposited and post deposition annealed films were amorphous. The surface morphology and topography of the films was studied using scanning electron microscopy and atomic force microscopy, respectively. A progressive decrease in the root mean square (RMS) roughness of the films from 1.53 nm to 0.7 nm was observed with increase in the annealing temperature. Al-Al2O3-Al thin film capacitors were then fabricated on p-type Si < 1 0 0 > substrate to study the effect of temperature and frequency on the dielectric property of the films and the results are discussed.

A transmission electron microscopy and X-ray photoelectron spectroscopy study of annealing induced gamma-phase nucleation, clustering, and interfacial dynamics in reactively sputtered amorphous alumina thin films

Pure alpha-Al2O3 exhibits a very high degree of thermodynamical stability among all metal oxides and forms an inert oxide scale in a range of structural alloys at high temperatures. We report that amorphous Al2O3 thin films sputter deposited over crystalline Si instead show a surprisingly active interface. On annealing, crystallization begins with nuclei of a phase closely resembling gamma-Alumina forming almost randomly in an amorphous matrix, and with increasing frequency near the substrate/film interface. This nucleation is marked by the signature appearance of sharp (400) and (440) reflections and the formation of a diffuse diffraction halo with an outer maximal radius of approximate to 0.23 nm enveloping the direct beam. The microstructure then evolves by a cluster-coalescence growth mechanism suggestive of swift nucleation and sluggish diffusional kinetics, while locally the Al ions redistribute slowly from chemisorbed and tetrahedral sites to higher anion coordinated sites. Chemical state plots constructed from XPS data and simple calculations of the diffraction patterns from hypothetically distorted lattices suggest that the true origins of the diffuse diffraction halo are probably related to a complex change in the electronic structure spurred by the a-gamma transformation rather than pure structural disorder. Concurrent to crystallization within the film, a substantially thick interfacial reaction zone also builds up at the film/substrate interface with the excess Al acting as a cationic source. (C) 2015 AIP Publishing LLC.

Effects of gamma-irradiation on Al2O3 crystals grown under reducing atmosphere

Gamma-ray irradiation-induced color centers in Al2O3 crystals grown by temperature gradient techniques (TGT) under a strongly reducing atmosphere were studied. The transition F+ -> F takes place during the irradiation process. Glow discharge mass spectroscopy (GDMS) and annealing treatments show that Fe3+ impurity ions are present in the crystals. A composite (F+-Fe3+) defect was presented to explain the origin of the 255 nm band absorption in the TGT-Al2O3 crystals. (C) 2006 Elsevier B.V. All rights reserved.

Effects of sapphire substrate annealing on ZnO epitaxial films grown by MOCVD

The annealing effects of sapphire substrate on the quality of epitaxial ZnO films grown by metalorganic chemical vapor deposition (MOCVD) were studied. The atomic steps formed on (0 0 0 1) sapphire (alpha-Al2O3) substrate surface by annealing at high temperature was analyzed by atomic force microscopy (AFM). The annealing effects of sapphire substrate on the ZnO films were examined by X-ray diffraction (XRD), AFM and photoluminescence (PL) measurements. Experimental results indicate that the film quality is strongly affected by annealing treatment of the sapphire substrate surface., The optimum annealing temperature of sapphire substrates is given. (c) 2006 Elsevier B.V. All rights reserved.