Preparation and characterization of ZnO-TiO2 films obtained by sol-gel method

The sol-gel route has been applied to obtain ZnO-TiO₂ thin films. For comparison, pure TiO₂ and ZnO films are also prepared from the corresponding solutions. The films are deposited by a spin-coated method on silicon and glass substrates. Their structural and vibrational properties have been studied as a function of the annealing temperatures (400-750 °C). Pure ZnO films crystallize in a wurtzite modification at a relatively low temperature of 400 °C, whereas the mixed oxide films show predominantly amorphous structure at this temperature. XRD analysis shows that by increasing the annealing temperatures, the sol-gel Zn/Ti oxide films reveal a certain degree of crystallization and their structures are found to be mixtures of wurtzite ZnO, Zn₂TiO₄, anatase TiO₂ and amorphous fraction. The XRD analysis presumes that Zn₂TiO₄ becomes a favored phase at the highest annealing temperature of 750 °C. The obtained thin films are uniform with no visual defects. The optical properties of ZnO-TiO₂ films have been compared with those of single component films (ZnO and TiO₂). The mixed oxide films present a high transparency with a slight decrease by increasing the annealing temperature.     

Influence of annealing on the physical properties of filtered vacuum arc deposited tin oxide thin films

Tin oxide (SnO₂) thin films were deposited on UV fused silica (UVFS) substrates using filtered vacuum arc deposition (FVAD). During deposition, the substrates were at room temperature (RT). As-deposited films were annealed at 400 and 600 °C in Ar for 30 min. The film structure, composition, and surface morphology were determined as function of the annealing temperature using X-ray diffraction (XRD), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The XRD patterns of the SnO₂ thin films deposited on substrates at RT indicated that the films were amorphous, however, after the annealing the film structure became polycrystalline. The grain size of the annealed films, obtained from the XRD analysis, increased with the annealing temperature, and it was in the range 8-34 nm. The AFM analysis of the surface revealed an increase in the film surface average grain size from 15 nm to 46 nm, and the surface roughness from 0.2 to 1.8 nm, as function of the annealing temperature. The average optical transmission of the films in the visible spectrum was >80%, and increased by the annealing ∼10%. The films’ optical constants in the 250-989 nm wavelength range were determined by variable angle spectroscopic ellipsometry (VASE). The refractive indexes of as-deposited and annealed films were in the range 1.83-2.23 and 1.85-2.3, respectively. The extinction coefficients, k(λ), of as-deposited and annealed films were in the range same range ∼0-0.5. The optical energy band gap (E_g), as determined by the dependence of the absorption coefficient on the photon energy at short wavelengths, increased with the annealing temperature from 3.90 to 4.35 eV. The lowest electrical resistivity of the as-deposited tin oxide films was 7.8 × 10⁻³ Ω cm, however, film annealing resulted in highly resistive films.     

Influence of annealing condition on the properties of sputtered hafnium oxide

Hafnium oxide thin films were deposited on p-type (1 0 0) silicon wafers by reactive dc magnetron sputtering. Prior to the deposition of HfO₂ films, a thin Hf film was deposited. Sputtered HfO₂ thin films deposited at room temperature remain amorphous at T<650°C and orthorhombic phases were observed above 650 °C. The monoclinic phase which is a stable HfO₂ polymorphic form appeared after annealing above 800 °C. Capacitance equivalent thickness values decreased and leakage characteristics are improved by the Hf interlayer and O₂ settlement process. The decrease of accumulation capacitance values upon annealing is due to the growth of an interfacial layer upon post-annealing. The flat band voltage (V_FB) shifts negatively due to positive charge generated during post-annealing.     

Electrical and corrosion properties of the Ti5Si3 thin films coated on glass substrate by APCVD method

Ti₅Si₃ thin films were coated on glass substrate by atmospheric pressure chemical vapor deposition method at different temperatures. Electrical and corrosion properties of the thin films were investigated. The results show that the electrical resistivity of the thin films decreases initially with the increase in deposition temperature. However, it increases with the further increase of the temperature. The lowest electrical resistivity of 107 μΩ⋅cm is obtained at 710 °C. The least corrosion rates of the thin films at 95 °C of 0.10 nm/min and 0.13 nm/min in 1 N and 10 N acid solution and of 0.33 nm/min and 6.55 nm/min in 1 N and 10 N alkali solution, respectively, are obtained by weight-loss measurement method. The corrosion mechanisms of the thin films were also discussed in detail.     

The effect of thermal annealing on the structural and mechanical properties of a-C:H thin films prepared by the CFUBM magnetron sputtering method

a-C:H films were prepared by closed-field unbalanced magnetron (CFUBM) sputtering on silicon substrates using argon (Ar) and acetylene (C₂H₂) gases, and the effects of post-annealing temperature on structural and mechanical properties were investigated. Films were annealed at temperatures ranging from 300 °C to 700 °C in increments of 200 °C using rapid thermal annealing equipment in vacuum ambient. Variations in microstructure were examined using Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Surface and mechanical properties were investigated by atomic force microscopy (AFM), nano-indentation, residual stress tester, and nano-scratch tester. We found that the mechanical properties of a-C:H films deteriorated with increased annealing temperature.     

The effects of annealing temperature on photoluminescence of silicon nanoparticles embedded in SiNx matrix

The effects of the annealing temperature on photoluminescence (PL) of non-stoichiometric silicon nitride (SiN_x) thin films deposited by plasma enhanced chemical vapor deposition (PECVD) using ammonia and silane mixtures at 200 °C were investigated. The optical property and the chemical composition of the films annealed at different temperatures were investigated by PL spectroscopy and Fourier transform infrared absorption spectroscopy (FTIR), respectively. Based on the PL results and the analyses of the bonding configurations of the films, the light emission is attributed to the quantum confinement effect of the carriers inside silicon nanoparticles and radiative defect-related states. These results provide a better understanding of optical properties of silicon nanoparticles embedded in silicon nitride films and are useful for the application of nanosize silicon semiconductor material.     

Growth of epitaxial TmFeCuO4 thin films by pulsed laser deposition

Epitaxial thin films of TmFeCuO₄ with a two-dimensional triangular lattice structure were successfully grown on yttria-stabilized-zirconia substrates by pulsed laser deposition and ex situ annealing in air. The films as-deposited below 500 °C showed no TmFeCuO₄ phase and the subsequent annealing resulted in the decomposition of film components. On the other hand, as-grown films deposited at 800 °C showed an amorphous nature. Thermal annealing converted the amorphous films into highly (0 0 1)-oriented epitaxial films. The results of scanning electron microscopic analysis suggest that the crystal growth process during thermal annealing is dominated by the regrowth of non-uniformly shaped islands to the distinct uniform islands of hexagonal base.     

Isothermal crystallization kinetic of ZnO thin films

Zinc oxide (ZnO) thin films deposited by DC magnetron sputtering were annealed in nitrogen atmosphere at different temperatures ranging from 100 to 500 °C with a step of 100 °C; the annealing time was 6 h. In order to study the film’s crystallization kinetic, their structures were monitored by means of X-ray diffraction (XRD) analysis each hour. Variation in grain size, calculated from the XRD patterns, with annealing time and temperature, obeys the classical parabolic law of grain growth. Exponent n was found to be dependent on the annealing temperature; it ranged from 5.13 to 3.8 with increase in annealing temperature. From the obtained exponent n values we inferred that the grain growth mechanism is mainly governed by the atom jumping across the grain boundary. We have found that the grain growth is characterized by a low activation energy ranging from 22 to 24 kJ/mol.     

Structure and growth morphology of Gd2O3-doped CeO2 thin films

Gd₂O₃-doped CeO₂ (Gd_0.1Ce_0.9O_1.95, GDC) thin films were synthesized on (1 0 0) Si single crystal substrates by a reactive radio frequency magnetron sputtering technique. Structures and surface morphologies were characterized by X-ray diffraction (XRD), Atomic Force Microscopy (AFM) and one-dimensional power spectral density (1DPSD) analysis. The XRD patterns indicated that, in the temperature range of 200–700 °C, f.c.c. structured GDC thin films were formed with growth orientations varying with temperature—random growth at 200 °C, (2 2 0) textures at 300–600 °C and (1 1 1) texture at 700 °C. GDC film synthesized at 200 °C had the smoothest surface with roughness of R_rms=0.973 nm. Its 1DPSD plot was characterized with a constant part at the low frequencies and a part at the high frequencies that could be fitted by the f^−2.4 power law decay. Such surface feature and scaling behavior were probably caused by the high deposition rate and random growth in the GDC film at this temperature. At higher temperatures (300–700 °C), however, an intermediate frequency slope (−γ₂≈−2) appeared in the 1DPSD plots between the low frequency constant part and the high frequency part fitted by f⁻⁴ power law decay, which indicated a roughing mechanism dominated by crystallographic orientation growth that caused much rougher surfaces in GDC films (R_rms>4 nm).     

Electrical, structural and optical properties of SnO2 thin films prepared by spray pyrolysis

This study investigated the effect of the substrate temperature on the structural, optical, morphological, and electrical properties of undoped SnO₂ films prepared by a spray deposition method. The films were deposited at various substrate temperatures ranging from 300-500 °C in steps of 50 °C and characterized by different optical and structural techniques. X-ray diffraction studies showed that the crystallite size and preferential growth directions of the films were dependent on the substrate temperature. These studies also indicated that the films were amorphous at 300 °C and polycrystalline at the other substrate temperatures used. Infrared and visible spectroscopic studies revealed that a strong vibration band, characteristic of the SnO₂ stretching mode, was present around 630 cm⁻¹ and that the optical transmittance in the visible region varied over the range 75-95% with substrate temperature, respectively. The films deposited at 400 °C exhibited the highest electrical conductivity property.     

Effects of rapid thermal treatments on the electrical properties of thin SiO2 gate oxide for DRAM p-channel MOS transistors

Silicon oxide has been grown by rapid thermal processing. The growth rate, in the range of very thin films (<10 nm), has been studied as a function of the oxidation temperature. Combined films composed by conventional thermal silicon oxide growth over SiO₂ passivation layer deposited by rapid thermal processing onto Si(1 0 0) substrates have been used as gate oxide of p-channel metal-oxide semiconductor (p-MOS) transistors of dynamic random access memory (DRAM). The effect of rapid thermal annealing treatments on these films has also been experimented. Improvements in the electrical performances of transistors have been observed.     

Growth of GaN films on PLD-deposited TaC substrates

GaN films were grown by metal organic chemical vapor deposition on TaC substrates that were created by pulsed laser deposition of TaC onto (0 0 0 1) SiC substrates at ∼1000 °C. This was done to determine if good quality TaC films could be grown, and if good quality GaN films could be grown on this closely lattice matched to GaN, conductive material. This was done by depositing the TaC on on-axis and 3° or 8° off-axis (0 0 0 1) SiC at temperatures ranging from 950 to 1200 °C, and examining them using X-ray diffraction, scanning electron microscopy, atomic force microscopy, and transmission electron microscopy. The GaN films were grown on as-deposited TaC films, and films annealed at 1200, 1400, or 1600 °C, and examined using the same techniques. The TaC films were polycrystalline with a slight (1 1 1) texture, and the grains were ∼200 nm in diameter. Films grown on-axis were found to be of higher quality than those grown on off-axis substrates, but the latter could be improved to a comparable quality by annealing them at 1200–1600 °C for 30 min. TaC films deposited at temperatures above 1000 °C were found to react with the SiC. GaN films could be deposited onto the TaC when the surface was nitrided with NH₃ for 3 min at 1100 °C and the low temperature buffer layer was AlN. However, the GaN did not nucleate easily on the TaC film, and the crystallites did not have the desired (0 0 0 1) preferred orientation. They were ∼10 times larger than those typically seen in films grown on SiC or sapphire. Also the etch pit concentration in the GaN films grown on the TaC was more than 2 orders of magnitude less than it was for growth on the SiC.     

Structure and optical characterization of photochemically prepared ZrO2 thin films doped with erbium and europium

Zirconium oxide thin films loaded with 10, 30 and 50 mol% lanthanide ions (Er or Eu) have been successfully prepared by direct UV (254 nm) irradiation of amorphous films of β-diketonate complexes on Si(1 0 0) substrates, followed by a post annealing treatment process. The resultant films were characterized by X-ray photoelectron spectroscopy and Atomic Force Microscopy. The results showed that the stoichiometry of the resulting films were in relative agreement with the composition of the precursor films. The effects of annealing as well as the lanthanide ion loading on the photoluminescence (PL) emission intensity were investigated, finding that thermal treatment decreases surface roughness as well as PL emission intensity.     

Structural and optical properties of 6CaO·6SrO·7Al2O3 thin films derived by sol-gel dip coating process

The nanostructured 6CaO·6SrO·7Al₂O₃ (C6S6A7) thin films with cubic structure using calcium, strontium metals, aluminium isopropoxide and ethylene glycol monomethyl ether as stating materials has been fabricated via sol-gel route. Based on hydrolysis of Ca²⁺, Sr²⁺ and Al³⁺ in the sol-gel processing using ethylene glycol monomethyl ether as solvent have been employed as the precursor material. The films were coated on soda lime float glass by the dip coating technique and annealed at 450 °C in air atmosphere. The structure, morphology and composition of the films were investigated by Fourier transformed infrared spectroscopy, X-ray powder diffraction, scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectroscopy indicating that the films were composed of C6S6A7 nanoparticles with cubic structure. The spectral transmittance of the films was measured in the wavelength range of 200-1100 nm using an UV-visible spectrometer. It has been found that the optical properties of the films significantly affected by precursor chemistry and annealing temperature due to the improvement of the crystallinity of the films with increasing annealing temperature and became stable when the annealing temperature is higher than 450 °C. The C6S6A7 films annealed at 450 °C had high transparency about 80% in wide visible range.     

Dependence of chemical composition and bonding of amorphous SiC on deposition temperature and the choice of substrate

Amorphous SiC has superior mechanical, chemical, electrical, and optical properties which are process dependent. In this study, the impact of deposition temperature and substrate choice on the chemical composition and bonding of deposited amorphous SiC is investigated, both 6 in. single-crystalline Si and oxide covered Si wafers were used as substrates. The deposition was performed in a standard low-pressure chemical vapour deposition reactor, methylsilane was used as the single precursor, and deposition temperature was set at 600 and 650 °C. XPS analyses were employed to investigate the chemical composition, Si/C ratio, and chemical bonding of deposited amorphous SiC. The results demonstrate that these properties varied with deposition temperature, and the impact of substrate on them became minor when deposition temperature was raised up from 600 °C to 650 °C. Nearly stoichiometric amorphous SiC with higher impurity concentration was deposited on crystalline Si substrate at 600 °C. Slightly carbon rich amorphous SiC films with much lower impurity concentration were prepared at 650 °C on both kinds of substrates. Tetrahedral Si-C bonds were found to be the dominant bonds in all deposited amorphous SiC. No contribution from Si-H/Si-Si but from sp² and sp³ C-C/C-H bonds was identified.     

Influence of hydrogen on structural and optical properties of low temperature polycrystalline Ge films deposited by RF magnetron sputtering

To improve the properties of polycrystalline Ge thin films, which are a candidate material for the bottom cells of low cost monolithic tandem solar cells, ∼300 nm in situ hydrogenated Ge (Ge:H) thin films were deposited on silicon nitride coated glass by radio-frequency magnetron sputtering. The films were sputtered in a mixture of 15 sccm argon and 10 sccm hydrogen at a variety of low substrate temperatures (T_s)≤450 °C. Structural and optical properties of the Ge:H thin films were measured and compared to those of non-hydrogenated Ge thin films deduced in our previous work. Raman and X-ray diffraction spectra revealed a structural evolution from amorphous to crystalline phase with increase in T_s. It is found that the introduction of hydrogen gas benefits the structural properties of the polycrystalline Ge film, sputtered at 450 °C, although the onset crystallization temperature is ∼90 °C higher than in those sputtered without hydrogen. Compared with non-hydrogenated Ge thin films, hydrogen incorporated in the films leads to broadened band gaps of the films sputtered at different T_s.     

Optical and electrical properties of lithium doped nickel oxide films deposited by spray pyrolysis onto alumina substrates

Non-doped and lithium doped nickel oxide crystalline films have been prepared onto quartz and crystalline alumina substrates at high substrate temperature (600 °C) by the pneumatic spray pyrolysis process using nickel and lithium acetates as source materials. The structure of all the deposited films was the crystalline cubic phase related to NiO, although this crystalline structure was a little bit stressed for the films with higher lithium concentration. The grain size had values between 60 and 70 nm, almost independently of doping concentration. The non-doped and lithium doped films have an energy band gap of the order of 3.6 eV. Hot point probe results show that all deposited films have a p-type semiconductor behavior. From current–voltage measurements it was observed that the electrical resistivity decreases as the lithium concentration increases, indicating that the doping action of lithium is carried out. The electrical resistivity changed from 10⁶ Ω cm for the non-doped films up to 10² Ω cm for the films prepared with the highest doping concentration.     

Structural relaxation of Al-W amorphous thin films

The pronounced variation of the electrical resistivity of the amorphous Al-W thin films observed during initial heating above room temperature was examined. Both isochronal and isothermal treatments were performed in order to investigate the effects of the film composition, substrate material, and substrate temperature, on the magnitude of the relaxation phenomena. Regarding the isochronal heating, it was observed that the relaxation effects decreased with an increase of the heating rate, and decreased with the aluminum content in the film. The Al₇₈W₂₂ amorphous thin films were subjected to isothermal annealing for 6 h at a temperature of 515 °C. The effects of the substrate material (alumina ceramic, glass and sapphire), and the deposition temperature (LNT, RT, 200 and 400 °C) were examined. The relaxation decreased in a sequence of: alumina ceramic-glass-sapphire substrates, as well as with an increase of the substrate temperature. An assumed dominant role of the aluminum in the effects observed, was tested by the corresponding investigation of Al-Ti and Cu-Ti amorphous thin films.     

Layer-by-layer growth and growth-mode transition of SrRuO3 thin films on atomically flat single-terminated SrTiO3 (1 1 1) surfaces

We report on growth-mode transitions in the growth of SrRuO₃ thin films on atomically flat Ti⁴⁺ single-terminated SrTiO₃ (1 1 1) substrates, investigated by reflection high-energy electron diffraction and atomic force microscopy. Over the first ~9 unit cells, the dominant growth mode changes from island to layer-by-layer for the growth rate of 0.074 unit cells/s and the growth temperature of 700 °C. Moreover, in the course of growing SrRuO₃ films, the governing growth mode of interest can be manipulated by changing the growth temperature and the growth rate, which change allows for the selection of the desired layer-by-layer mode. The present study thus paves the way for integrations of SrRuO₃ thin layers into (1 1 1)-orientated oxide heterostructures, and hence multi-functional devices, requiring control of the sharp atomic-level interfaces and the layer-by-layer growth mode.