Stresses in sputtered RUOx thin films

RuO_x thin films have been deposited by reactive sputtering in an O₂/Ar atmosphere. The films were characterized for their stress and resistivity as a function of deposition temperature (room temperature, 300°C) and the O₂ content (25–100%) in the sputtering gas. Additionally, the stresses in these films were determined as a function of annealing temperature (up to 600°C) using an in-situ curvature measurement technique. The as-deposited films were found to be under a state of compressive stress for all deposition conditions. The compressive stresses sharply increased with increasing deposition temperature from a value of around 200 MPa at 200°C to 1400 MPa at 300°C. This dramatic increase has been attributed to differences in microstructure at these deposition temperatures. The microstructural differences also led to the widely differing stress-temperature behavior during annealing of these films. For films deposited at temperatures lower than 200°C, the annealing process resulted in a decrease in the compressive stress and resistivity of the films. However, films deposited at a temperature of 300°C did not show any changes in the compressive stress or resistivity after annealing. The results of this study can be used to deposit RuO_x thin films with low resistivity and minimal stresses.     

Thermal stability and crystallization kinetics of sputtered amorphous Si3N4 films

The crystallization of thin silicon nitride (Si₃N₄) films deposited on polycrystalline SiC substrates was investigated by X-ray diffractometry as a function of annealing time. The amorphous Si₃N₄ films were produced by means of reactive r.f. magnetron sputtering. Annealing at temperatures between 1300 and 1700 °C led to the formation of crystalline films composed of -Si₃N₄ and β-Si₃N₄. The fraction of β-Si₃N₄ in the films reaches approximately 40% at temperatures above 1550 °C. Both polymorphic modifications were formed simultaneously during the crystallization process. A transformation of -Si₃N₄ to β-Si₃N₄ could not be observed in the time and temperature range investigated. The crystallization process of amorphous Si₃N₄ can be described according to the Johnson–Mehl–Avrami–Kolmogorov (JMAK) formalism, assuming a three-dimensional, interface controlled grain growth from pre-existing nuclei. The rate constants show an Arrhenius behaviour with an activation enthalpy of approximately 5.5 eV.     

Strong magnetoelastic effect in Pr1−xCaxMnO3

Manganese oxides with distorted perovskite structure have attracted much attention during the last decade due to their colossal magnetoresistance (CMR), and the strong correlations among the various degrees of freedom involved. In particular, Pr_1−xCa_xMnO₃ compounds present in a wide Ca-doping range a charge ordering phenomenon, consisting of real space ordering of Mn³⁺ and Mn⁴⁺ in alternate lattice sites below a certain temperature T_CO. This ordering brings about a lattice distortion and a large hardening of the sound velocity below T_CO. Tomioka et al. have observed that an applied magnetic field can melt this charge ordered state and induce a transition from an insulating to a metallic state. In order to study the effects of this charge order melting, ultrasonic longitudinal sound velocity measurements were performed on polycrystalline Pr_1−xCa_xMnO₃ (x=0.35 and 0.5) as a function of magnetic field and temperature. Interesting anomalies were found related to the melting of the charge ordered phase into a metal-like state even at low temperatures.     

Phase formation process of IrxSi1−x thin films Structure and electrical properties

Experimental data on the phase formation process of amorphous Ir_xSi_1−x thin films with 0.30 ≤ x ≤ 0.41 are presented and discussed in relation to electric transport properties. The structure formation process at temperatures from 300 K up to 1223 K was investigated by means of X-ray diffraction. Distinct phases were observed in the final stage in dependence on the initial composition: Ir₃Si₄, Ir₃Si₅, and IrSi₃. An unknown metastable phase was found in films with a silicon concentration of 61 at.% to 64 at.% after annealing above the crystallization temperature T = 970 K. The crystal structure of this phase was determined by the combined use of X-ray diffraction and electron diffraction. It was found to be monoclinic, basic-face centred with lattice constants a = 1.027 nm, b = 0.796 nm, c = 0.609 nm, and γ = 113.7°. Additionally, microstructure and morphology of the films were investigated by transmission electron microscopy (TEM). The annealing process was studied by means of mechanical stress investigations as well as by electrical resistivity and thermopower measurements. Correlations between the structure, the phase formation and the electrical transport behaviour are discussed on the basis of conduction mechanism.     

Synthesis of boron-doped diamond films by DC plasma CVD using a CH4+CO2+H2 gas mixture at lower substrate temperature and formation of an n-Si/p-diamond heterojunction

Diamond films were synthesized by direct current plasma chemical vapour deposition using a CH₄+CO₂+H₂ gas mixture on Si substrates. The optimum deposition conditions were determined. It was found that 0.4 A/cm² current density, at applied voltage of 1 kV, resulted in good-quality diamond films. The substrate temperature was 750 K which is considerably lower than the conventional requirement of ∼1100 K. Boron doping was achieved by passing a portion of the gas mixture through boric acid dissolved in methanol. The boron-doped p-type diamond films were deposited on an n-type single crystalline Si substrate and an n-Si/p-diamond heterojunction was fabricated. The p-n junction was characterized in terms of current-voltage (I-V) and capacitance-voltage (C-V) measurements.     

Impact of substrate temperature on the microstructure, electrical and optical properties of sputtered nanoparticle V2O5 thin films

Applying reactive direct current (DC) magnetron sputtering method, nanoparticle vanadium pentoxide thin films were deposited onto glass slides and KBr substrates at different substrate temperatures. The films were characterized by X-ray photoelectron spectroscopy and atomic force microscope. Infrared spectra were recorded with a Fourier transform infrared spectrophotometer. It was found that, excepting the compositions, the film growth and vanadium oxygen bonds were strongly affected by the substrate temperature. Electrical measurements indicated that the square resistances of films showed an exponential decrease from 46 MΩ/□ to 33 kΩ/□ with substrate temperature increasing from 433 K to 593 K, and that the square resistance-temperature curves of films exhibited typical semiconducting behavior. Optical investigations were carried out in the near infrared and ultraviolet-visible range. Transmittance varied from about 95 to 55% in near-infrared range when the substrate temperature was elevated. In ultraviolet-visible range, optical band gaps and refractive indexes of films were deduced according to the transmission and reflection spectra.     

Relationship between photoluminescence and structural properties of the sputtered Zn1−xCdxO films on Si substrates

Zn_1−xCd_xO (x=0.2, 0.4) alloyed crystal thin films have been deposited on Si(1 1 1) substrates at different temperatures by using dc reactive magnetron sputtering technique. The Zn_1−xCd_xO films are of highly (0 0 2)-preferred orientation possessing the hexagonal wurtzite structure of pure ZnO. At 450 °C, the films have better crystal quality and photoluminescent characteristics. For the films with x=0.2 and 0.4, the corresponding near-band-edge (NBE) energies are 3.10 and 3.03 eV, respectively, both have red-shifts compared with that of ZnO (3.30 eV). For the substrate temperatures lower or higher than 450 °C, the other NBE emission peak appears, the X-ray diffraction intensity of (0 0 2) peak decreases and the related FWHM increases. With the Cd addition up to x=0.4 both the XRD and PL intensity of the Zn_1−xCd_xO films decrease sharply in comparison with x=0.2.     

Current noise in MgB2 superconducting thin films

In this paper we present some experimental results concerning the current noise produced during the resistive transition in MgB₂ thin films. Preliminary investigations evidenced the presence of electrical noise whose power spectrum has a region of the 1/fⁿ type with n 3. We suggest that the noise may originate from abrupt rearrangement of the current distribution inside the specimen during the percolative process of a diphasic system. Experimental measurements of the spectral components of the current noise taken during the resistive transition will be given and discussed.     

Structure and mechanical properties of DC magnetron sputtered TiC/Cu films

TiC/Cu nanocomposite films with various copper content were deposited by DC unbalanced magnetron sputtering from sintered TiC target fixed by Cu rings of different inner diameters in pure argon. This makes it possible to prepare TiC/Cu films with Cu content ranging from approximately 5 to 85 at% Cu. The structure (XRD, Raman, SEM) and mechanical properties were examined as a function of deposition parameters and Cu content in the film. Special attention is devoted to the total internal stress, parameters determining its magnitude and their correlation with mechanical properties. The TiC/Cu system is compared with similar nitride MeN_x/Cu(Ni) (Me=Ti, Zr) systems and an explanation of the different behavior of nitride and carbide systems is proposed.     

Physical properties of flash evaporated In2O3 films prepared at different substrate temperatures

Indium oxide (In₂O₃) thin films were prepared by flash evaporated technique under various substrate temperatures in the range of 303-673 K and systematically studied the structural, electrical and optical properties of the deposited films. The films formed at substrate temperatures of < 373 K were amorphous while those deposited at higher substrate temperatures (≥ 373 K) were polycrystalline in nature. The optical band gap of the films decreased from 3.71 eV to 2.86 eV with the increase of substrate temperature from 303 K to 673 K. Figure of merit of the films increased from 2.8 × 10³ Ω^− 1 cm^− 1 to 4.2 × 10³ Ω^− 1 cm^− 1 with increasing substrate temperature from 303 K to 573 K, thereafter decreased to 2.2 × 10³ Ω^− 1 cm^− 1 at higher temperature of 673 K.     

Flux pinning in high-Tc superconductive films

Magnetization measurements have been performed onc-axis oriented Y- and Gd-based superconductive films in a wide range of the temperaturesT (4.2–85 K) and magnetic fieldsH (0–8 T) withH c-axis. The influence of flux creep on both the temperature dependence of critical current densityJ _cm and the scaling behavior of flux pinning forceF _p has been discussed in detail. The experimental results show that Y and Gd films have different pinning mechanism. Flux pinning-force peaks in high fields are observed in Gd film at high temperatures and can be considered as evidence for collective pinning.     

Investigation on the structure of TiO2 films sputtered on alloy substrates

Titanium dioxide (TiO₂) films have been successfully deposited on metal alloy substrates by radio-frequency magnetron reactive sputtering in an Ar+O₂ gas mixture. The effects of gas total pressure on the structure and phase transition of TiO₂ films were studied by X-ray diffraction and Raman spectra. It is suggested that the film structure changes from rutile to anatase while work gas total pressure changes from 0.2 to 2 Pa. The structure of TiO₂ films is not affected by the film thickness.     

The inherent optical nonlinearities of thin silver films

Thin Ag films with the thickness of 80 Å were prepared by pulsed laser deposition technique. The films were grown on MgO(1 0 0) substrates under the nitrogen pressure of 5.0 Pa at room temperature. The surface images of the films were observed by atomic force microscopy. The linear optical properties of the films were studied in the wavelength range of 300–800 nm. The inherent third-order nonlinear optical responses coming from the silver material itself were determined by z-scan method at the wavelength of 532 nm with laser duration of 10 ns. The significant optical nonlinearities of the pure thin Ag films were determined to have the real and imaginary parts of the third-order nonlinear optical susceptibility (χ⁽³⁾) as 2.49 × 10⁻⁸ and 7.16 × 10⁻⁹ esu, respectively. The obtained χ⁽³⁾ value of Ag films was about one order of magnitude larger than that of Ag colloids.     

Competition between dislocation nucleation and void formation as the stress relaxation mechanism in passivated Cu interconnects

We perform systematic calculations to study the competition between the dislocation nucleation and void formation as stress relaxation mechanism in Cu interconnects under thermal stress, which is related to the aspect ratio (ratio of the film thickness to width) of the Cu lines. It is quantitatively found from both elastic-perfectly plastic model and kinematic strain hardening model that there exists a critical aspect ratio, below and above which the stress relaxation is dominated by the dislocation nucleation and void formation, respectively. The critical aspect ratio is revealed to modulate by both the length scale of the interconnects and the interfacial strength between the Cu lines and surroundings, suggesting potential application to achieve artificial controlling on stress relaxation mechanism in Cu lines. Calculations are in good agreement with available experiments.     

Determination of the E1 and E1+Δ1 energy bands by photoreflectance in AlxGa1−xAs in the region 0<x<0.55

The E₁ and E₁+Δ₁ energy bands of metal–organic chemical vapor deposition grown Al_xGa_1−xAs, with x in the range 0–0.55, have been determined using photoreflectance technique. The aluminum composition for each sample was determined using the energy of the room-temperature photoluminescence compensated peak value and a suitable fundamental band gap formula. The positions of the E₁ and E₁+Δ₁ peaks were determined from curve-fitting an appropriate theoretical model to our experimental data by a modified downhill simplex method. Using the results, we propose new E₁ and E₁+Δ₁ cubic expressions as functions of the aluminum composition, x, and compare them with the available reported expressions.     

Preparation of Pt-PtOx thin films as electrode for memory capacitors

Pt-PtO_x thin films were prepared on Si(100) substrates at temperatures from 30 to 700°C by reactive r.f. magnetron sputtering with platinum target. Deposition atmosphere was varied with O₂/Ar flow ratio. The deposited films were characterized by X-ray diffraction, X-ray photoelectron spectroscopy and scanning electron microscopy. Resistively of the deposited films was measured by d.c. four probe method. The films mainly consisted of amorphous PtO and Pt₃O₄ (or Pt₂O₃) below 400°C, and amorphous Pt was increased in the film as a deposition temperature increased to 600°C. When deposition temperature was thoroughly increased, (111) oriented pure Pt films were formed at 700°C. Compounds included in the films strongly depended on substrate temperature rather than O₂/Ar flow ratio. Electrical resistivity of Pt-PtO_x films was measured to be from the order of 10⁻¹ Ω cm to 10⁻⁵ Ω cm, which was related to the amount of Pt phase included in the deposited films.     

Amplitude-dependent internal friction in copper thin films on silicon substrates

Internal friction in copper thin films 0.2–1.5 μm thick on silicon substrates has been measured between 180 and 340 K as a function of strain amplitude. Analysis of the amplitude-dependent internal friction in the copper films shows the relation between the plastic strain of the order of 10⁻⁹ and the effective stress on dislocation motion. The stress–strain curves thus obtained for the copper films tend to shift to a higher stress with decreasing film thickness and also with decreasing temperature, both indicating a suppression of microplastic flow. It is concluded that the microflow stress at a constant level of the plastic strain varies inversely with the film thickness at all temperatures examined. The film thickness effect in the microplastic range can be explained on the basis of a dislocation-bowing model.     

Preparation and characterization of LiNiVO4 powder and non-stoichiometric LiNixVyOz films

Inverse spinel type structured oxide, LiNiVO₄, was synthesized by using solid-state method and the crystalline powder was characterized by Rietveld refinement and X-ray photoelectron spectroscopy. Non-stoichiometric lithium nickel vanadate thin films were prepared by physical vapour deposition technique. The amorphous films were characterized by Rutherford back-scattering spectroscopy (RBS), nuclear reaction analysis (NRA), Auger electron spectroscopy (AES), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) analytical methods. Films crystal growth at various temperatures was also studied by XRD and SEM. The HRTEM analysis of sputtered film shows nanocrystalline domains of NiO and LiNiVO₄ phases with characteristic lattice parameters of the host compound and the results correlate well with the XRD data. Electrochemical properties of the films were discussed.     

Structural relaxation and crystallisation of bulk metallic glasses Zr41Ti14Cu12.5Ni10−xBe22.5Fex (x = 0 or 2) studied by mechanical spectroscopy

The measurements of the internal friction and dynamic shear modulus as well as differential scanning calorimetry have been performed in order to investigate the structural relaxation and crystallization of Zr₄₁Ti₁₄Cu_12.5Ni_10−xBe_22.5Fe_x (x=0 or 2) bulk metallic glasses. It is found that the glass transition is retarded and the thermal stability of supercooled liquid is increased by the Fe addition. The experimental results are well analyzed using a physical model, which can characterize atomic mobility and mechanical response of disordered condensed materials.     

Relaxation peaks associated with the oxygen-ion diffusion in La2−xBixMo2O9 oxide-ion conductors

The effects of bismuth doping on the oxygen-ion diffusion in oxide-ion conductors La_2−xBi_xMo₂O₉ (x=0.05, 0.1, and 0.15) have been studied by both internal friction and dielectric relaxation techniques. Two internal friction peaks of relaxation type (P₁ and P₂ peak) were observed at a measurement frequency of 4 Hz around 380 and 430 K, respectively. As for the dielectric measurement, a prominent dielectric relaxation peak (P_d) was found in all the Bi-doped samples around 700 K at a measurement frequency of 50 kHz, which actually consists of two sub-peaks (denoted as P_d1 and P_d2 peak). With increasing Bi-doping content, two peaks shift to higher temperature and decrease in height, while the activation energy of both peaks increases. The main reason was interpreted as the introduction of the lone-pair electrons of bismuth, which tends to block the diffusion of oxygen ion.