An investigation of structural phase transformation and electrical resistivity in Ta films

In this work, we report the effect of substrate, film thickness and sputter pressure on the phase transformation and electrical resistivity in tantalum (Ta) films. The films were grown on Si(1 0 0) substrates with native oxides in place and glass substrates by varying the film thickness (t) and pressure of the working gas (p_Ar). X-ray diffraction (XRD) analysis showed that the formation of α and β phases in Ta films strongly depend on the choice of substrate, film thickness t and sputter pressure p_Ar. A stable α-phase was observed on Si(1 0 0) substrates for t ≤ 200 nm. Both α and β phases were found to grow on glass substrates at all thicknesses except t = 100 nm. All the films grown on Si(1 0 0) substrates for p_Ar ≤ 6.5 mTorr had α-phase with strong (1 1 0) texture normal to the film plane. The glass substrates promoted the formation of β-phase in all p_Ar except p_Ar = 5.5 mTorr. The resistivity ρ was observed to decrease with t, whereas ρ was increased with p_Ar on Si(1 0 0) substrates. In all films, the measured resistivity ρ was greater than the bulk resistivity. The resistivity ρ was influenced by the effects of surface roughness and grain size.     

Structural and magnetic properties of evaporated Fe thin films on Si(1 1 1), Si(1 0 0) and glass substrates

We present experimental results on the structural and magnetic properties of series of Fe thin films evaporated onto Si(1 1 1), Si(1 0 0) and glass substrates. The Fe thickness, t, ranges from 6 to110 nm. X-ray diffraction (XRD) and atomic force microscopy (AFM) have been used to study the structure and surface morphology of these films. The magnetic properties were investigated by means of the Brillouin light scattering (BLS) and magnetic force microscopy (MFM) techniques. The Fe films grow with (1 1 0) texture; as t increases, this (1 1 0) texture becomes weaker for Fe/Si, while for Fe/glass, the texture changes from (1 1 0) to (2 1 1). Grains are larger in Fe/Si than in Fe/glass. The effective magnetization, 4πM_eff, inferred from BLS was found to be lower than the 4πM_S bulk value. Stress induced anisotropy might be in part responsible for this difference. MFM images reveal stripe domain structure for the 110 nm thick Fe/Si(1 0 0) only.     

Structure of PtFe/Fe double-period multilayers investigated by X-ray diffraction, reflectivity, diffuse scattering and TEM

Double-period [(Pt 1.7 nm/Fe 0.9 nm)₅Fe(t_Fe2)]₈ and [(Pt 1.8 nm/Fe 0.6 nm)₅Fe(t_Fe2)]₈ multilayers with different thickness t_Fe2 (between 0.23 and 4.32 nm) of the additional Fe layers, prepared by combinatorial sputter deposition, show differences in the mosaic spread and the vertical interfacial roughness when deposited on native or thermally oxidised Si wafers. Simulations of the wide-angle X-ray scattering intensities revealed the presence of interdiffusion in the (Pt/Fe)₅ bilayers and systematic variations of the grain sizes, perpendicular to the film surface, as well as the rms variations of the two superlattice periods with the total film thickness. A comparison of ω-rocking scans shows an increase of the correlated vertical roughness of the (Pt/Fe)₅ multilayers with the total multilayer thickness.     

Metal organic chemical vapor deposition of ultrathin ZrO2 films on Si(1 0 0) and Si(1 1 1) studied by electron spectroscopy

The growth of ultrathin ZrO₂ films on Si(1 0 0)-(2 × 1) and Si(1 1 1)-(7 × 7) has been studied with core level photoelectron spectroscopy and X-ray absorption spectroscopy. The films were deposited sequentially by chemical vapor deposition in ultra-high vacuum using zirconium tetra-tert-butoxide as precursor. Deposition of a > 50 Å thick film leads in both cases to tetragonal ZrO₂ (t-ZrO₂), whereas significant differences are found for thinner films. On Si(1 1 1)-(7 × 7) the local structure of t-ZrO₂ is not observed until a film thickness of 51 Å is reached. On Si(1 0 0)-(2 × 1) the local geometric structure of t-ZrO₂ is formed already at a film thickness of 11 Å. The higher tendency for the formation of t-ZrO₂ on Si(1 0 0) is discussed in terms of Zr-O valence electron matching to the number of dangling bonds per surface Si atom. The Zr-O hybridization within the ZrO₂ unit depends furthermore on the chemical composition of the surrounding. The precursor t-butoxy ligands undergo efficient C-O scission on Si(1 0 0), leaving carbonaceous fragments embedded in the interfacial layer. In contrast, after small deposits on Si(1 1 1) stable t-butoxy groups are found. These are consumed upon further deposition. Stable methyl and, possibly, also hydroxyl groups are found on both surfaces within a wide film thickness range.     

Structural studies of evaporated CoxCr1−x/Si (1 0 0) and CoxCr1−x/glass thin films

Series of Co_xCr_1−x thin films have been evaporated under vacuum onto Si (1 0 0) and glass substrates. Chemical composition and interface properties have been studied by modelling Rutherford backscattering spectra (RBS) using SIMNRA programme. Thickness ranges from 17 to 220 nm, and x from 0.80 to 0.88. Simulation of the energy spectra shows an interdiffusion profile in the thickest films, but no diffusion is seen in thinner ones. Microscopic characterizations of the films are done with X-ray diffraction (XRD) measurements. All the samples are polycrystalline, with an hcp structure and show a 〈0 0 0 1〉 preferred orientation. Atomic force microscopies (AFM) reveal very smooth film surfaces.     

Effect of growth parameters on the structure and magnetic properties of thin polycrystalline Fe films fabricated on Si〈1 0 0〉 substrates

This paper deals with the experimental investigation of the structure and magnetic properties of thin polycrystalline Fe films. Two sets of 50 ± 2 nm thick Fe films were fabricated on Si〈1 0 0〉 substrates with native oxides in place by varying (i) the sputter pressure p_Ar and (ii) the Fe sputter power P_Fe. X-ray diffraction (XRD) study revealed that all films grew with strong 〈1 1 0〉 texture normal to the film plane. No higher order peaks were observed in any of the films studied. For both film sets, the lattice constant (a) was less than the bulk Fe lattice constant (a₀ = 2.866 Å), which suggested the existence of compressive strain in all films. Two regions of homogeneous strain were observed over the range of p_Ar studied. Magneto-optical Kerr effect (MOKE) measurements showed that all films exhibited magnetically isotropic behaviour. The magnetic properties were observed to be influenced strongly by p_Ar. The film grown at p_Ar = 4 μbar was the most softest (H_s = 100 ± 8 kA m⁻¹, M_r/M_s = 0.87 ± 0.02) film among all the films studied. The magnetic properties were found to be independent of P_Fe. The effective saturation magnetostriction constant λ_eff determined (using the Villari method) was positive (4 ± 1 ppm) and observed to vary within the calculated error.     

Thickness-dependent magnetization reversal in CoZrNb amorphous films

Structure and magnetization of CoZrNb amorphous films prepared by DC magnetron sputtering have been studied as a function of film thickness (t), from 35 to 840 nm. Using comprehensive characterization, we show that the CoZrNb amorphous films possess a single phase and no nanocrystalline can be detected. The magnetic measurements indicate that the magnetization reversal of CoZrNb films is strongly dependent on t. That is, the coercivity is abruptly reduced to be lower than 4 Oe with t increasing from 35 to 105 nm, and then gradually decreases to ∼0.2 Oe as t increases. This coercivity transition versus t is accompanied by the strong magnetization reversal when t is larger than 105 nm. The results reveal that CoZrNb amorphous films with comparatively large film thickness (>100 nm) are suitable for sensors and anti-faked materials.     

Microstructure and magnetic properties studies of SmCo5 thin films grown on MgO and glass substrates

In this work, SmCo₅ thin films are deposited on single crystal MgO (1 0 0) and amorphous glass substrates with a Cr underlayer at 400 °C by sputtering. A comparison study shows that the microstructures and magnetic properties are different in the two SmCo₅ films on the MgO (1 0 0) and glass substrates, respectively. An epitaxial growth of Cr-(2 0 0)〈1 1 0〉/SmCo₅-(1 1 2¯ 0)〈0 0 0 1〉 is achieved on the MgO (1 0 0) single crystal substrate with an average grain size of 20 nm for SmCo₅. On the amorphous glass substrate, no significant crystallographic texture is found in the Cr underlayer. After the deposition of SmCo₅, a weak texture of (1 1 2¯ 0) is observed with an average grain size of 8 nm. High remanence ratio value in this film is probably due to strong exchange coupling. Both SmCo₅ films show high in-plane coercivity, high in-plane anisotropy and remanence enhancement.     

Structure, magnetic and electrical transport properties of cosputtered Fe0.5Ge0.5 nanocomposite films

Fe_0.5Ge_0.5 nanocomposite films with different film thicknesses were fabricated using cosputtering. The films are composed of Ge, Fe and Fe₃Ge₂, and are ferromagnetic at room temperature. The saturation magnetization and magnetic interaction including dipolar interaction and exchange coupling increase with the increasing film thickness. The electrical conductance mechanism turns from metallic to semiconducting and the saturation Hall resistivity ρ_xys increases with the decreasing film thickness. At 28 nm, ρ_xys is ∼137 μΩ cm at 2 K, about 150 times larger than that of pure Fe film (0.9 μΩ cm) and four orders larger than that of bulk Fe. The ρ_xy-H curves of all the films show the same linearity character in low-field range even though the temperature-independent slope is different at different film thicknesses. At high temperatures, the skew scattering mechanism is dominant. At low temperatures, side-jump effect should be dominant at large resistivity ρ_xx regime for the thin films, and the skew scattering is dominant at small ρ_xx regime for the thick films.     

Magnetic properties of strontium hexaferrite films prepared by pulsed laser deposition

The magnetic properties of strontium hexaferrite (SrFe₁₂O₁₉) films fabricated by pulsed laser deposition on the Si(100) substrate with Pt(111) underlayer have been studied as a function of film thickness (50–700 nm). X-ray diffraction patterns confirm that the films have c-axis perpendicular orientation. The coercivities in perpendicular direction are higher than those for in-plane direction which indicates the films have perpendicular magnetic anisotropy. The coercivity was found to decrease with increasing of thickness, due to the increasing of the grain size and relaxation in lattice strain. The 200 nm thick film exhibits hexagonal shape grains of 150 nm and optimum magnetic properties of M_s=298 emu/cm³ and H_c=2540 Oe.     

Preparation and characterization of transparent NiO thin films deposited by spray pyrolysis technique

Nickel oxide thin films were successfully fabricated with various deposition time (t_d = 5, 10, and 15 min) on glass substrates using spray pyrolysis technique. The deposited films undergo thermal treatment at 350 °C for various annealing time (t_a = 0, 15, 30 and 60 min). In this study, the effect of t_d and t_a on film thickness was observed and their influence on structural, morphological and optical properties were investigated. The films deposited with t_d = 5 min showed amorphous structure while the films grown at higher deposition time became partially crystallized with preferred growth along (1 1 1) direction. Heat treatment carried out in air allowed us to tune the polycrystalline structure and the diffraction intensity at preferred peak increases with the increase in t_a which is a consequence of better crystallinity. This was reflected in the AFM micrographs of the films which suggested that the thermal annealing (or increasing t_a) facilitates the process of grain-growth, and improves the crystalline microstructure. The optical transmission of the films was found to vary with t_d and t_a and thus film thickness. The thinner films show higher transparency in the UV–vis spectral region. The optical band gap was blue-shifted from 3.35 eV to 3.51 eV depending on t_a. The effect of t_a on the various optical constants of the NiO films has also been discussed.     

Structure, magnetic and magnetostrictive properties of as-deposited Fe-Ga thin films

Polycrystalline Fe_100−xGa_x (19?x?23) films were grown on Si(1 0 0) substrates at different partial pressures of sputtering gas ranging from 3 to 7 μbar. Microstructural, magnetic and magnetostrictive properties were studied using X-ray diffraction (XRD), atomic force microscopy (AFM), energy dispersive spectroscopy (EDS) and magneto-optic Kerr effect (MOKE) magnetometry respectively. X-ray diffraction showed that all films have the body-centered cubic (bcc) Fe-Ga phase with the 〈1 1 0〉 direction out of the film plane. Magnetic characterization of the films showed that the films prepared at 3 μbar had weak uniaxial anisotropy whereas films grown at Ar pressures in the range 4-7 μbar were magnetically isotropic. The effective saturation magnetostriction constants (λ_eff) of the films were measured using the Villari effect. It was found that effective saturation magnetostriction constants were almost constant over the Ga composition range achieved by varying the sputtering pressure. The measured effective magnetostriction constants fit closely to the calculated saturation magnetostriction constants of 〈1 1 0〉 textured polycrystalline films with the 〈1 1 0〉 directions slightly canted with respect to the normal to the sample surface. It was found that a high pressure of the sputtering gas effected the magnetic softness of the films. The saturation field increased and remanence ratio decreased with increase in pressure.     

Nanostructuring of Fe films by oblique incidence deposition on a FeSi2 template onto Si(1 1 1): Growth, morphology, structure and faceting

The growth of thin Fe films deposited at oblique incidence on an iron silicide template onto Si(1 1 1) single crystal has been investigated as a function of Fe thickness (0 < t_Fe ? 180 monolayers (MLs)) and incidence angle (0 ? θ ? 80°). The growth mode is determined in situ by means of scanning tunnelling microscopy (STM) and low energy electron diffraction (LEED). Stripes oriented perpendicularly to the incident atomic flux are formed for θ ? 30°. Self-correlation functions are used to extract characteristic lengths from STM images. The correlation lengths in the direction of the incident flux (ξ_x) and perpendicular to the atomic flux (ξ_y) grow with different powers versus time (ξ_x∝t^σ and ξ_y∝t^ρ, with σ = 0.34 ± 0.03 and ρ = 0.67 ± 0.03) following the exact solution of the (1 + 1) dimensional Kardar-Parisi-Zhang (KPZ) equation. The root mean square roughness follows also a scaling law for t_Fe < 120 ML leading to a growth exponent β = 0.73 ± 0.02. Shadowing and steering effects are discussed on the basis of our STM data.     

Non-hysteretic metal-insulator transition of VO2 films grown by excimer-laser-assisted metal organic deposition process

We examined the correlation between thickness of an epitaxial VO₂ phase grown on a TiO₂ (0 0 1) substrate by the excimer-laser-assisted metal organic deposition (ELAMOD) process and the metal-insulator transition (MIT) property of it. The abrupt and hysteretic MIT was observed for the epitaxial films (thickness: t ≥ 6 nm), and the epitaxial film (t ≤ 4 nm) showed semiconductor behavior. When an amorphous VO_x layer was prepared on the ultrathin epitaxial phase (t ≤ 4 nm) by the ELAMOD, a non-hysteretic MIT was successfully observed. The non-hysteretic MIT was found to be owing to roughened interface between the epitaxial phase and the amorphous phase, where there would be a number of structural defects.     

Fabrication and characterization of sputtered titanium dioxide films

TiO₂ thin films were prepared under various conditions by using a reactive RF sputtering technique. The structural, optical and electrical characteristics of the films have been investigated. All as-deposited films were amorphous. After annealing at T > 673 K, the crystallinity of the observed tetragonal anatase phase appeared improved. The optical band gap, determined by using Tauc plot, has been found to amount to 3.38 ± 0.03 and 3.21 ± 0.03 eV for the direct and indirect transition, respectively. Also the complex optical constants for the wavelength range 300-2500 nm are reported. Using the two-point probe technique, the dark resistivity has been measured as a function of the film thickness, d. The resistivity, ρ, of the samples has been found to decrease markedly with increasing thickness, but only for d < 100 nm. The behaviour of ρd versus d was found to fit properly with the Fuchs and Sondheimer relation with parameters ρ_o = 4.95 × 10⁶ Ω cm and mean free path, l = 310 ± 2 nm. The log ρ versus 1/T curves show three distinct regions with values for the activation energy of 0.03 ± 0.01, 0.17 ± 0.01 and 0.50 ± 0.02 eV, respectively.     

Role of crystal orientation on the magnetic properties of CoFe2O4 thin films grown on Si (1 0 0) and Al2O3 (0 0 0 1) substrates using pulsed laser deposition

We report the influence of crystal orientation on the magnetic properties of CoFe₂O₄ (CFO) thin films grown on single crystal Si (1 0 0) and c-cut sapphire (Al₂O₃) (0 0 0 1) substrates using pulsed laser deposition technique. The thickness was varied from 200 to 50 nm for CFO films grown on Si substrates, while it was fixed at 200 nm for CFO films grown on Al₂O₃ substrates. We observed that the 200 and 100 nm thick CFO-Si films grew in both (1 1 1) and (3 1 1) directions and displayed out-of-plane anisotropy, whereas the 50 nm thick CFO-Si film showed only an (1 1 1) orientation and an in-plane anisotropy. The 200 nm thick CFO film grown on an Al₂O₃ substrate was also found to show a complete (1 1 1) orientation and a strong in-plane anisotropy. These observations pointed to a definite relation between the crystalline orientation and the observed magnetic anisotropy in the CFO thin films.     

Growth dynamics of pulsed laser deposited indium oxide thin films: a substrate dependent study

Indium oxide films are deposited by pulsed laser deposition in the presence of oxygen atmosphere, on different substrates, namely GaAs, Si, quartz, and glass. The structural, morphological, and interface characteristics are studied. Cubic In₂O₃ phase is confirmed by high resolution X-ray diffraction measurements. While the films on Si, glass, and quartz substrates are polycrystalline, the films on GaAs exhibit a preferred orientation along (2 2 2) plane. The structure and crystalline nature of the films are also confirmed by Raman spectroscopy. Furthermore, Raman spectra show the appearance of gallium oxide modes arising due to Ga diffusion from the substrate. The morphology of the films deposited on different substrates is studied by atomic force microscopy and rms roughness values are obtained. A two-dimensional power spectral density analysis has been used to calculate the growth exponent (α). A value of α > 1 (α < 1) for films grown on GaAs/Si (quartz/glass) substrates suggests that the growth on crystalline substrates is governed by the linear diffusion model, whereas the growth on amorphous substrates follows the dynamic scaling behaviour. UV-visible study shows a high optical transmittance of >90% and a band gap value of 3.64 and 3.79 eV for the films deposited on quartz and glass substrates, respectively.     

Laser synthesis of semiconductor nanostructures with narrow band gap

Semiconductor nanostructures with narrow band gap were synthesized by means of laser chemical vapor deposition (LCVD) of elements from iron carbonyl vapors [Fe(CO)₅] under the action of Ar⁺ laser radiation (λ_L = 488 nm) on the Si substrate surface. The temperature dependence of the specific conductivity of these nanostructures in the form of thin films demonstrated typical semiconductor tendency and gave the possibility to calculate the band gap for intrinsic conductivity (E_g) and the band gap assigned for impurities (E_i), which were depended upon film thickness and applied electrical field. Analysis of deposited films with scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrated their cluster structure with average size not more than 100 nm. Semiconductor properties of deposited nanostructures were stipulated with iron oxides in different oxidized phases according to X-ray photoelectron spectroscopy (XPS) analysis.These deposited nanostructures were irradiated with Q-switched YAG laser (λ_L = 1064 nm) at power density about 6 × 10⁷ W/cm². This irradiation resulted in the crystallization process of deposited films on the Si substrate surface. The crystallization process resulted in the synthesis of iron carbide-silicide (FeSi_2−xC_x) layer with semiconductor properties too. The width of the band gap E_g of the synthesized layer of iron carbide-silicide was less than for deposited films based on iron oxides Fe₂O_3−x (0 ≤ x ≤ 1).     

Epitaxial growth and optical characterization of compound semiconductor β-FeSi2 prepared by pulsed laser deposition

β-FeSi₂ thin films were prepared on FZ n-Si (1 1 1) substrates by pulsed laser deposition (PLD). The structural properties and crystallographic orientation of the films were investigated by X-ray diffraction (XRD) analysis. This indicates that β-FeSi₂/Si (2 0 2/2 2 0) and the single-crystalline β-FeSi₂ can be prepared using PLD. In photoluminescence (PL) measurements at 8 K detected by Ge detector, the PL spectra of the samples annealed at 900 °C for 1, 5, 8 and 20 h showed that the PL intensity of the A-band peak increased depending on annealing time in comparison with those of as-deposited samples. The intrinsic PL intensity of the A-band peak at 0.808 eV of the β-FeSi₂ from the 20-h-annealed sample was investigated for the first time by the PLD method detected by an InGaAs detector. This result has been confirmed by temperature dependence and excitation power density of the 20-h-annealed sample with the comparison of other defect-related band peaks of the sample. Cross-sectional scanning electron microscopy (SEM) observation was also performed and the thickness of the thin films was found to be at 75 nm for 20-h-annealed. The thermal diffusion for the epitaxial growth of β−FeSi₂/Si was observed when the compositional ratio of Fe to Si was around Fe:Si=1:2 for 20-h-annealed carried out by energy dispersive X-ray spectroscopy (EDX). We discussed high crystal quality of the epitaxial growth and optical characterization of β-FeSi₂ achieved after annealing at 900 °C for 20 h.     

Thickness measurement of a thin hetero-oxide film with an interfacial oxide layer by X-ray photoelectron spectroscopy

The general equation T_ove = L cos  θ ln(R_exp/R₀ + 1) for the thickness measurement of thin oxide films by X-ray photoelectron spectroscopy (XPS) was applied to a HfO₂/SiO₂/Si(1 0 0) as a thin hetero-oxide film system with an interfacial oxide layer. The contribution of the thick interfacial SiO₂ layer to the thickness of the HfO₂ overlayer was counterbalanced by multiplying the ratio between the intensity of Si⁴⁺ from a thick SiO₂ film and that of Si⁰ from a Si(1 0 0) substrate to the intensity of Si⁴⁺ from the HfO₂/SiO₂/Si(1 0 0) film. With this approximation, the thickness levels of the HfO₂ overlayers showed a small standard deviation of 0.03 nm in a series of HfO₂ (2 nm)/SiO₂ (2-6 nm)/Si(1 0 0) films. Mutual calibration with XPS and transmission electron microscopy (TEM) was used to verify the thickness of HfO₂ overlayers in a series of HfO₂ (1-4 nm)/SiO₂ (3 nm)/Si(1 0 0) films. From the linear relation between the thickness values derived from XPS and TEM, the effective attenuation length of the photoelectrons and the thickness of the HfO₂ overlayer could be determined.