Thickness-dependent properties of sprayed iridium oxide thin films

Iridium oxide thin films with variable thickness were deposited by spray pyrolysis technique (SPT), onto the amorphous glass substrates kept at 350 °C. The volume of iridium chloride solution was varied to obtain iridium oxide thin films with thickness ranging from 700 to 2250 Å. The effect of film thickness on structural and electrical properties was studied. The X-ray diffraction (XRD) studies revealed that the as-deposited samples were amorphous and those annealed at 600 °C for 3 h in milieu of air were polycrystalline IrO₂. The crystallinity of Ir-oxide films ameliorate with film thickness thereby preferred orientation along (1 1 0) remains unchanged. The infrared spectroscopic results show Ir–O and Ir–O₂ bands. The room temperature electrical resistivity (ρ_RT) of these films decreases with increase in film thickness. The p-type semiconductor to metallic transition was observed at 600 °C.     

Alkoxide route to La0.5Sr0.5CoO3 epitaxial thin films on SrTiO3

An all alkoxide based sol–gel route was investigated for preparation of epitaxial La_0.5Sr_0.5CoO₃ (LSCO) films on 100 SrTiO₃ (STO) substrates. Films with 20–30 to 80–100 nm thickness were prepared by spin-coating 0.2–0.6 M (metal) solutions on the STO substrates and heat treatment to 800 °C at 2 °C min^− 1, 30 min, in air. The films were epitaxial with a cube-on-cube alignment and the LSCO cell was strained to match the STO substrate of 3.905 Å closely; a and b = 3.894 Å and 3.897 Å for the 20–30 and 80–100 nm films, respectively. The c-axis was compressed to 3.789 Å and 3.782 Å for the 20–30 and 80–100 nm films, respectively, which resulted in an almost unchanged cell volume as compared to polycrystalline film and nano-phase powders prepared in the same way. The SEM study showed mainly very smooth, featureless surfaces, but also some defects. A film prepared in the same way on an -Al₂O₃ substrate was dense and polycrystalline with crystallite sizes in the range 10–50 nm and gave cubic cell dimensions of a_c = 3.825 Å. The conductivity of the ca 30–40 nm thick polycrystalline film was 1.7 mΩcm, while the epitaxial 80–100 nm film had a conductivity of around 1.9 mΩcm.     

Studies using AFM and STM of the correlated effects of the deposition parameters on the topography of gold on mica

A systematic study of the correlated effects of deposition temperature, film thickness and deposition rate on the morphology of gold films on mica was carried out using atomic force microscopy and scanning tunnelling microscopy. For the range of thicknesses, rates and temperatures concerned, a variety of surface structures, mainly in the form of rounded mounds, islands, long channel and short channel plateaux topographical features were formed under various combinations of these three parameters. The rounded mounds and islands formed, respectively, on the mica substrate at room temperature and at 150°C were found to be essentially independent of the film thickness and deposition rate selected. When deposited at higher temperatures (300°C and 440°C), a change from islands to channelled features, via the growth and coalescence of the islands, was observed either on increasing the film thickness for a given deposition rate (≈ 1.0 Å s⁻¹) or on increasing the deposition rate to a given film thickness (400 Å). It is evident from the results presented that, whereas the film thickness and the deposition rate at a given temperature determine to what extent the film has coalesced, the growth temperature influences the lateral size of the surface features formed. In consequence, conducting films were found when the gold coverage was ≥ ≈0.9. Investigation of the vertical characteristics of the films was also conducted. The origin of all the phenomena observed can be attributed to competition between secondary nucleation and thermally enhanced diffusion processes occurring on the gold surface during deposition and film formation.     

Annealing effects on the thermoelectric power of thin copper and silver films

The effect of annealing on the thermoelectric power of thin copper and silver films has been investigated. Using Matthiessen's rule, the thermoelectric power is separated into three components: S₀ due to bulk lattice scattering, S_s due to surface scattering and S_i due to scattering by imperfections. The values of S₀ and S_s are independent of the film thickness, whereas S_i varies with film thickness. However, S_i approaches a constant value for both copper and silver when the film thickness is larger than 1000 Å. The values of S_s obtained for copper and silver films are 1.33 μV/°K and 3.23 μV/°K respectively. For thicker films (t>1000 Å), the values of S_i for copper and silver films are 3.89 μV/°K and 9.63 μV/°K respectively.     

IR spectra and etch rates of plasma-enhanced chemically vapour-deposited phosphosilicate glass films

IR transmission spectra of phosphosilicate glass (PSG) films with 8 wt.% P prepared by plasma-enhanced chemical vapour deposition (PECVD) and CVD are compared. The differential IR spectrum of a PECVD PSG film differs from that of a CVD PSG film: the P=O peak has a lower intensity than the corresponding peak of the CVD film with the same phosphorus content; no peaks are evident at 980 and 500 cm⁻¹—the characteristic frequencies for P---O---P stretching and bending vibrations. The differential IR spectra of PECVD and CVD PSG films become very similar after annealing for 4 h in water vapour at 850°C. The etch rate of a PECVD film in p-etchant, which is constant throughout the film thickness, is 400 Å min⁻¹. However, the etch rate recorded after the film is subjected to annealing in water vapour at 850°C varies with the depth in the film, attaining values as high as 800 Å min⁻¹ in the region near the outer surface of the film. The results are explained as due to the oxidation of P₂O₃ to P₂O₅.     

Effects of annealing temperature on the optical, bonding, structural and electrical properties of nitrogenated amorphous carbon thin films grown by surface wave microwave plasma chemical vapor deposition

We have studied the effects of annealing temperature (AT) on the properties of nitrogenated amorphous carbon (a-C:N) films grown at room temperature (RT) on quartz substrates by surface wave microwave plasma chemical vapor deposition (SWMP-CVD) using camphor alcohol gas as carbon plasma sources. The thickness, optical, bonding, structural and electrical properties of the as-grown (RT) and anneal-treated in range from 100 to 500°C of a-C:N films were measured and compared. The film thickness is decreased rapidly with increasing AT above 350°C. The wide range of optical absorption characteristics is observed depending on the AT. The optical band gap of as-grown a-C:N films is approximately 2.8 eV, gradually decreased to 2.5 eV for the films anneal-treated at 300°C and beyond that it decreased rapidly up to 0.9 eV at 500°C . Visible-Raman Spectroscopy (Raman) revealed the amorphous structure of as-grown a-C:N films and, the growth of nanocrystallinity of a-C:N films upon increase of AT. Raman and Fourier transform infrared spectroscopy (FTIR) analyses respectively shown the structural and composition of the films can be tuned by optimizing the AT. The change of optical, bonding, structural and electrical properties of SWMP-CVD grown a-C:N films with higher AT was attributed due to the fundamental changes in the bonding and band structure of the a-C:N films.     

Mechanical properties of a-C:H and a-C:H/SiOx nanocomposite thin films prepared by ion-assisted plasma-enhanced chemical vapor deposition

a-C:H and a-C:H/SiO_x nanocomposite thin films were deposited on silicon, aluminum and polyimide substrates at 25 °C in an asymmetric 13.56 MHz r.f.-driven plasma reactor under heavy ion bombardment. Fourier transform infrared spectra of the films indicate that the nanocomposite filmsappears to consist of an atomic scale random network of a-C:H and SiO_x. Raman spectroscopy revealed that the sp² carbon fraction in the nanocomposite film was reduced compared with the a-C:H film. The intrinsic stress of both films increased with increasing negative bias voltage (−V_dc) at the substrate. However, the nanocomposite films exhibited lower intrinsic stress compared w with a-C:H-only films. Especially, a thin SiO_x-rich interlayer was very effective in reducing the film stress and enhancing the bonding strength at the interface. The interlayer allowed deposition of thick films of up to 5 μm. Also, the nanocomposite films were stable in 0.1 M NaOH solution and showed good microhardness.     

Effects of substrate on the structural, electrical and optical properties of Al-doped ZnO films prepared by radio frequency magnetron sputtering

Transparent and conductive Al-doped ZnO (AZO) thin films were deposited on substrates including alkali-free glass, quartz glass, Si, and SiO₂ buffer layer on alkali-free glass by using radio frequency magnetron sputtering. The effects of different substrates on the structural, electrical and optical properties of the AZO films were investigated. It was found that the crystal structures were remarkably influenced by the type of the substrates due to their different thermal expansion coefficients, lattice mismatch and flatness. The AZO film (100 nm in thickness) deposited on the quartz glass exhibited the best crystallinity, followed sequentially by those deposited on the Si, the SiO₂ buffer layer, and the alkali-free glass. The film deposited on the quartz glass showed the lowest resistivity of 5.14 × 10^− 4 Ω cm among all the films, a carrier concentration of 1.97 × 10²¹ cm^− 3 and a Hall mobility of 6.14 cm²/v·s. The average transmittance of this film was above 90% in the visible light spectrum range. Investigation into the thickness-dependence of the AZO films revealed that the crystallinity was improved with increasing thickness and decreasing surface roughness, accompanied with a decrease in the film resistivity.     

Ni-Al2O3 selective cermet coatings for photothermal conversion up to 500°C

Spectrally selective Ni-Al₂O₃ composite films were prepared by r.f. planar magnetron sputtering using hot-pressed targets of two different compositions. The composition of the films were varied by co-sputtering the target with additional nickel pellets distributed uniformly on the target. The composition of the films were analysed by energy-dispersive X-ray analysis. Optical simulations were carried out with the experimentally measured n and k and the published n and k of the metallic substrate. R.f.-sputtered SiO₂ and Al₂O₃ were used as antireflection coatings. From the computer optimization studies we found that = 0.94 and (100°C) = 0.07 could be obtained with 650 Å of Ni-Al₂O₃ (f = 0.61) antireflected with 780 Å SiO₂ on a nickel-coated glass substrate. When molybdenum-coated nickel-plated stainless steel substrates were used, the films were found to be stable up to 500°C in air.     

Spray pyrolysis deposition of polycrystalline magnesia films and their use as buffer layers in Bi(Pb)-Sr-Ca-Cu-O/MgO/Al2O3 (or glass ceramics) structures

The deposition of MgO films on Al₂O₃ and glass ceramic substrates by spray pyrolysis of a water-ethanol magnesium nitrate precursor solution has been studied. Dense polycrystalline films have been obtained by repeated pyrolysis at 300–350 °C followed by annealing of the deposit in air at 970 °C. It has been established that the finest grains obtained under these experimental conditions correspond to the films deposited on glass ceramic substrates. It has been shown that the MgO films can be useful buffer layers preventing the interaction between the above substrates and the BiSr-Ca-Cu-O films deposited on them by spray pyrolysis of nitrates.     

Catalytic CVD growth and properties of a-C:H and a-C:N

Hydrogenated amorphous carbon (a-C:H) and nitrided amorphous carbon (a-C:N) films have been synthesized on quartz substrates at a substrate temperature of 700 °C using a catalytic chemical vapor deposition (Cat-CVD) method. Raman spectra of a-C:H films showed two principal bands, the G-band at 1600 cm⁻¹ and the D-band at 1350 cm⁻¹. Those of a-C:N films showed similar spectra, with a G′ band at 1640 cm⁻¹, the peak energy of which is higher than that of the G-band in a-C:H. The intensity ratio /I_D, which is a measure of the degree of order in a-C:H, decreased for a-C:H with increasing CH₄/H₂ gas-flow ratio. On the contrary, the /I_D ratio increased with increasing CH₄/H₂ gas-flow ratio.     

Sur la dispersion de l''anisotropie et de la stabilité dans le temps des couches électrolytiques de Ni-Fe-Mo avec anisotropie biaxiale

The angular and amplitude dispersions of the anisotropy in Ni-Fe-Mo films with biaxial anisotropy have been studied. The permalloy films had a thickness of 5000 Å and those of permalloy with 5% Mo a thickness of 5400 å. The films were deposited onto plane copper substrates. The angular and amplitude dispersions, measured by the resonance absorption method, decrease with an increase in the angle between the anisotropy axes, having values of 4° and 2.8 Oe, respectively, for the permalloy films with an angle of 5° between the axes, and 2° 30′ and 2 Oe for films with an angle of 22° between the axes. For the permalloy films with Mo the dispersions decrease from 7° 30′ and 3.2 Oe to 6° 30′ and 2.9 Oe for an increase of the angle between the anisotropy axes from 10° to 20°.

The time variation (over 1000 h) of the angle between the anisotropy axes is given. Decreases from 22° to 17° and from 10° to 7° respectively for permalloy and permalloy with 5% Mo are obtained.     

Anomalous photovoltaic effect in vacuum-deposited CdTe films

CdTe films of thicknesses varying from 125 to 1250 nm were vapour deposited onto glass substrates at oblique incidence in vacuum at substrate temperatures varying from room temperature to 250 °C. The samples are irradiated with an He-Ne laser from the direction of the deposited layer and through the substrate. It was found that the film thickness and substrate temperature play an important role in changing the magnitude and polarity of the photovoltages generated in CdTe films. A reversal in the polarity of the photovoltage is obtained in certain films depending on the deposition parameters. An attempt is made to interpret the results.     

Hydrothermal synthesis of β-nickel hydroxide nanocrystalline thin film and growth of oriented carbon nanofibers

Novel well-crystallized β-nickel hydroxide nanocrystalline thin films were successfully synthesized at low temperature on the quartz substrates by hydrothermal method, and the oriented carbon nanofibers (CNFs) were prepared by acetylene cracking at 750 °C on thin film as the catalyst precursor. High resolution transmission electron microscopy (HR-TEM) measurement shows that thin films were constructed mainly with hexagonal β-nickel hydroxide nanosheets. The average diameter of the nanosheets was about 80 nm and thickness about 15 nm. Hydrothermal temperature played an important role in the film growth process, influencing the morphologies and catalytic activity of the Ni catalysts. Ni thin films with high catalytic activity were obtained by reduction of these Ni(OH)₂ nanocrystalline thin films synthesized at 170 °C for 2 h in hydrothermal condition. The highest carbon yield was 1182%, and was significantly higher than the value of the catalyst precursor which was previously reported as the carbon yield (398%) for Ni catalysts. The morphology and growth mechanism of oriented CNFs were also studied finally.     

A three-step process for epitaxial growth of (111)-oriented C60 films on alkali–halide substrates

Epitaxial (111)-oriented C₆₀ films have been grown on alkali–halide substrates, KCl (100), KBr (100) and NaCl (100) by a three-step process: (1), substrate surface cleaning by high temperature heating; (2), initial deposition with a low deposition rate to grow two or three monolayers (ML); and (3), deposition with a high deposition rate to grow a film with expected thickness. It was found that (111)-oriented epitaxial C₆₀ films could be grown at low temperatures in a wide temperature range, from 40 to 120°C. By this three-step process, we can also grow epitaxial C₆₀ films at deposition rates as high as 35 Å/min.     

Morphological changes induced by thermal anneals in NiFe/Ag multilayers; their relation to the resistive and magnetoresistive properties

(Ti, Al)N films have drawn much attention as alternatives for TiN coatings, which are oxidized easily in air above 500 °C. We have investigated the effect of Al content on the oxidation resistance of (Ti_{1 − x}Al_x)N films prepared by r.f. reactive sputtering.

(Ti_{1 − x}Al_xN films (O ≤ x ≤ 0.55) were deposited onto fused quartz substrates by r.f. reactive sputtering. Composite targets with five kinds of Al-to-Ti area ratio were used. The sputtering gas was Ar (purity, 5 N) and N₂ (5 N). The flow rate of Ar and N₂ gas was kept constant at 0.8 and 1.2 sccm, respectively, resulting in a sputtering pressure of 0.4 Pa. The r.f. power was 300 W for all experiments. Substrates were not intentionally heated during deposition. The deposited films (thickness, 300 nm) were annealed in air at 600 900 °C and then subjected to X-ray diffractometer and Auger depth profiling.

The as-deposited (Ti_{1 − x}Al_x)N films had the same crystal structure as TiN (NaCl type). Al atoms seemed to substitute for Ti in lattice sites. The preferential orientation of the films changed with the Al content of the film, x. Oxide layers of the films grew during annealing and became thicker as the annealing temperature increased. The thickness of the oxide layer grown on the film surface decreased with increasing Al content in the film. For high Al content films an Al-rich oxide layer was grown on the surface, which seemed to prevent further oxidation. All of the films, however, were oxidized by 900 °C annealing, even if the Al content was increased up to 0.55.     

Chemical vapor deposition of aluminum from methylpyrrolidine alane complex

Chemical vapor deposition of aluminum from a recently developed precursor, methylpyrrolidine alane complex, has been studied. Aluminum films deposited on conducting surfaces (titanium nitride, copper, gold), but not on insulating surfaces (silicon, silicon dioxide, glass) at low substrate temperatures, showing deposition selectivity, while the deposition selectivity was lost at high substrate temperatures (> 210 °C). Al deposition rates on TiN and Cu were very close, but much higher than on Au. Deposition rates on all conducting substrates increased with the temperature and reached maximum at 180 °C. Al films deposited on as-sputtered TiN or Cu have no preferred orientations. Al–Au alloys and intermetallics were observed in the films deposited on Au. Surface morphology observation revealed that the film growth on TiN or Cu is different from that on Au. The surface roughness of Al films increased with the deposition time or the film thickness.     

Characterization of titanium dioxide atomic layer growth from titanium ethoxide and water

Atomic layer growth of titanium dioxide from titanium ethoxide and water was studied. Real-time quartz crystal microbalance measurements revealed that adsorption of titanium ethoxide is a self-limited process at substrate temperatures 100–250°C. A relatively small amount of precursor ligands was released during titanium ethoxide adsorption while most of them was exchanged during the following water pulse. At temperatures 100–150°C, incomplete reaction between surface intermediates and water hindered the film growth. Nevertheless, the deposition rate reached 0.06 nm per cycle at optimized precursor doses. At substrate temperatures above 250°C, the thermal decomposition of titanium ethoxide markedly influenced the growth process. The growth rate increased with the reactor temperature and titanium ethoxide pulse time but it insignificantly depended on the titanium ethoxide pressure. Therefore reproducible deposition of thin films with uniform thickness was still possible at substrate temperatures up to 350°C. The films grown at 100–150°C were amorphous while those grown at 180°C and higher substrate temperature, contained polycrystalline anatase. The refractive index of polycrystalline films reached 2.5 at the wavelength 580 nm.     

Yttrium oxide based metal-insulator-semiconductor structures on silicon

Yttrium oxide based metal-insulator-semiconductor (MIS) structures on silicon have been studied. Yttrium films of thickness of nearly 200 Å were deposited by electron beam evaporation on silicon substrates held at room temperature. The oxidation of yttrium was performed at 750 °C for 1 h in dry oxygen. Scanning electron microscopy showed a smooth surface morphology for oxidized films. X-ray diffraction analyses were also performed, but did not confirm the crystalline nature of the oxide. Capacitance-voltage and current-voltage measurements were conducted to characterize aluminum-yttrium oxide-silicon MIS structures. The results have demonstrated the potential of using yttrium oxide as a gate dielectric.     

Transparent conducting F-doped SnO2 thin films grown by pulsed laser deposition

Transparent conducting fluorine-doped tin oxide (SnO₂:F) films have been deposited on glass substrates by pulsed laser deposition. The structural, electrical and optical properties of the SnO₂:F films have been investigated as a function of F-doping level and substrate deposition temperature. The optimum target composition for high conductivity was found to be 10 wt.% SnF₂ + 90 wt.% SnO₂. Under optimized deposition conditions (T_s = 300 °C, and 7.33 Pa of O₂), electrical resistivity of 5 × 10^− 4 Ω-cm, sheet resistance of 12.5 Ω/□, average optical transmittance of 87% in the visible range, and optical band-gap of 4.25 eV were obtained for 400 nm thick SnO₂:F films. Atomic force microscopy measurements for these SnO₂:F films indicated that their root-mean-square surface roughness ( 6 Å) was superior to that of commercially available chemical vapor deposited SnO₂:F films ( 85 Å).