Growth control of RF magnetron sputtered SrRuO3 thin films through the thickness of LaNiO3 seed layers

SrRuO₃ (SRO) thin films were grown on SiO₂/Si substrates with different thickness of LaNiO₃ (LNO) seed layers by RF magnetron sputtering. Effects of LNO thickness on the grain orientation, surface morphology, magnetic behavior and electrical transport properties of SRO films were investigated. The orientation of SRO films transformed from (110)_pc to (001)_pc and the residual stress was released gradually with increasing the thickness (pc refers to the pseudo-cubic unit cell of SrRuO₃). SRO films with higher orientation grown on LNO exhibited more flat surface, higher saturation magnetization, and lower coercive field. The magnetic anisotropy was enhanced on thicker LNO due to the different states of residual stress. In addition, the temperature dependence of resistivity was promoted by the microstructural disorder. (110)_pc-oriented SRO monolayer electrode and (001)_pc-oriented SRO/LNO300 bilayer electrode own low room temperature sheet resistance of 0.38 Ω/□ and 0.26 Ω/□, respectively. The results indicate that the controllable SRO films can be used as not only good bottom electrodes but also promising templates to control the crystallographic orientations of various other perovskite-based functional materials.     

Si diffusion induced adhesion and corrosion resistance in annealed RF sputtered SiC films on graphite substrate

Silicon carbide (SiC) is one of the promising candidates for graphite protection in different applications involving high temperatures and a highly corrosive environment. An ideal Silicon carbide coating should withstand a corrosive environment without compromising its adhesion. Herein, RF magnetron sputtered silicon-rich SiC thin films were deposited on a graphite substrate followed by annealing at 1000 °C, 1200 °C, and 1400 °C in an inert atmosphere. The impact of annealing temperature on microstructure, adhesion and chemical stability of SiC thin films was demonstrated. Different analytical techniques like Scanning electron microscopy (SEM), X-Ray Diffraction (XRD), Fourier's Transform Infrared (FTIR) spectroscopy and nano-indentation were used to study microstructural evaluation and mechanical characteristics. Moreover, the electrochemical analysis (Tafel and Electrochemical impedance spectroscopy) was performed in 3.5% NaCl solution. The microstructural analysis revealed that the amorphous SiC thin film turned into a crystalline and dense film upon annealing. Scanning electron micrographs showed that silicon-rich regions at SiC film surface started to disappear as Si diffuses into graphite matrix at elevated temperatures. Both these factors contributed to improvement in the adhesion of SiC coating with graphite substrate as annealing temperature increased. In addition, the nano-indentation hardness of 5.2 GPa was obtained for as grown sample, which decreased at 1000 °C, and then increased at 1200 °C and 1400 °C. Furthermore, the electrochemical analysis confirmed the enhancement in corrosion resistance upon annealing at a temperature of 1200 °C and 1400 °C due to Si diffusion and film compactness in these samples.     

Microwave dielectric and nonlinear optical studies on radio‐frequency sputtered Dy2O3‐doped KNN thin films

We report the effect of oxygen mixing percentage (OMP) on structural, microstructural, dielectric, linear, and nonlinear optical properties of Dy₂O₃‐doped (K_0.5Na_0.5)NbO₃ thin films. The (K_0.5Na_0.5)NbO₃ + 0.5 wt%Dy₂O₃ (KNN05D) ferroelectric thin films were deposited on to quartz and Pt/Ti/SiO₂/Si substrates by RF magnetron sputtering. An increase in the refractive index from 2.08 to 2.21 and a decrease in the optical bandgap from 4.30 to 4.28 eV indicate the improvement in crystallinity, which is also confirmed from Raman studies. A high relative permittivity (ε_r=281‐332) and low loss tangent (tanδ=1.2%‐1.9%) were obtained for the films deposited in 100% OMP, measured at microwave frequencies (5‐15 GHz). The leakage current of the films found to be as low as 9.90×10^?9 A/cm² at 150 kV/cm and Poole‐Frenkel emission is the dominant conduction mechanism in the films. The third order nonlinear optical properties of the KNN05D films were investigated using modified single beam z‐scan method. The third order nonlinear susceptibility (?χ⁽³⁾?) values of KNN05D films increased from 0.69×10^?3 esu to 1.40×10^?3 esu with an increase in OMP. The larger and positive nonlinear refractive index n₂=7.04×10^?6 cm²/W, and nonlinear absorption coefficient β=1.70 cm/W were obtained for the 100% OMP film, indicating that KNN05D films are good candidates for the applications in nonlinear photonics and high‐frequency devices.     

Structural and optical properties of ZnS thin films deposited by RF magnetron sputtering

Zinc sulfide [ZnS] thin films were deposited on glass substrates using radio frequency magnetron sputtering. The substrate temperature was varied in the range of 100°C to 400°C. The structural and optical properties of ZnS thin films were characterized with X-ray diffraction [XRD], field emission scanning electron microscopy [FESEM], energy dispersive analysis of X-rays and UV-visible transmission spectra. The XRD analyses indicate that ZnS films have zinc blende structures with (111) preferential orientation, whereas the diffraction patterns sharpen with the increase in substrate temperatures. The FESEM data also reveal that the films have nano-size grains with a grain size of approximately 69 nm. The films grown at 350°C exhibit a relatively high transmittance of 80% in the visible region, with an energy band gap of 3.79 eV. These results show that ZnS films are suitable for use as the buffer layer of the Cu(In, Ga)Se₂ solar cells.     

Effects of NIR annealing on the characteristics of al-doped ZnO thin films prepared by RF sputtering

Aluminum-doped zinc oxide (AZO) thin films have been deposited on glass substrates by employing radio frequency (RF) sputtering method for transparent conducting oxide applications. For the RF sputtering process, a ZnO:Al₂O₃ (2 wt.%) target was employed. In this paper, the effects of near infrared ray (NIR) annealing technique on the structural, optical, and electrical properties of the AZO thin films have been researched. Experimental results showed that NIR annealing affected the microstructure, electrical resistance, and optical transmittance of the AZO thin films. X-ray diffraction analysis revealed that all films have a hexagonal wurtzite crystal structure with the preferentially c-axis oriented normal to the substrate surface. Optical transmittance spectra of the AZO thin films exhibited transmittance higher than about 80% within the visible wavelength region, and the optical direct bandgap (E_g) of the AZO films was increased with increasing the NIR energy efficiency.     

Investigation into the effect of substrate material on microstructure and optical properties of thin films deposited via magnetron sputtering technique

This study aims at investigating the effect of the substrate material on growth mechanism and also microstructure of Ta₂O₅ thin films. For this purpose, atomic force microscopy, scanning electron microscopy, and interferometry analyses were implemented to reveal the influence of silicon wafer and amorphous BK7 glass substrates on the nucleation and growth mechanisms of Ta₂O₅ thin films deposited via the radio frequency magnetron sputtering technique. Results indicated that those films with finer morphologies had relatively higher nucleation densities. Compared with BK7 glass substrate, crystals formed on the silicon wafer were shown to be finer and had lower mean areas in more nucleation sites. Moreover, optical properties and morphological characteristics of the films on the silicon substrates had much more endurance after the annealing treatment. It was observed that shift in the transmission spectra of the deposited films after the treatment was insignificant, implying high packing density of the films. However, a 6-nm shift in the transmission spectra indicated low density and high porosity of the films. Finally, atomic force microscopy analysis along with the light scattering measurements confirmed the formation of a low-roughness film on the silicon wafer substrates.     

Effect of Fe-doping on the structural,optical and magnetic properties of ZnO thin films prepared by RF magnetron sputtering

In this paper, we report the fabrication and systematic characterization of Fe Doped ZnO thin Films. Fe_xZn_1−x O (x=0<0.05) films were prepared by RF magnetron sputtering on Si (400) substrate. Influence of Fe doping on structural, optical and magnetic properties has been studied. The X-ray diffraction (XRD) analysis shows that Fe doping has affected the crystalline structure, grain size and strain in the thin films. The best crystalline structure is obtained for 3% Fe Doping as observed from Atomic Force Microscopy (AFM) and X-ray diffraction (XRD). The magnetic properties studied using Vibrating Sample Magnetometer reveals the room temperature ferromagnetic nature of the thin films. However, changing the Fe concentration degrades the magnetic property in turn. The mechanism behind the above results has been discussed minutely in this paper.     

Structure,electrical, optical and magnetoelectric properties of magnetron sputtered nanocrystalline NiFe/BaTiO3 thin films

BaTiO₃ (BTO) and NiFe films grown on SrTiO₃ (STO), Nb:SrTiO₃ (NSTO), and ITO-glass substrates were prepared by radio-frequency (RF) and direct-current (DC) magnetron sputtering, respectively. The microstructure, ferroelectricity, leakage current, magnetoelectric (ME) coupling, ultraviolet–visible light spectrum, optical band gap, ellipsometry spectrum and surface morphology of the composite film are characterized by XRD, ferroelectric analyzer, ME coupling test system, U-4100, Horiba Smart SE and AFM. In addition, the stress, strain and piezoelectric voltage of the magnetoelectric composite film under the action of DC and AC magnetic fields are simulated by COMSOL multiphysics software. The experimental results show that the prepared composite film is polycrystalline, the surface roughness of the film is better, and the particles are uniform. The magnetoelectric coupling voltage gradually increases with the increase of the value of the DC magnetic field and the frequency of the AC magnetic field, and it has a larger absorption (about 0.3) at 340 nm. In addition, the simulation results also show the relationship between the coupling voltage V_ME and the applied magnetic field H.     

Magnetic studies on one-step chemically synthesized nickel ferrite thin films

Nickel ferrite thin films were synthesized at room temperature using one-step electrodeposition solution processing. Reaction kinetics was also proposed. An effect of air baking on the structural, surface morphological and magnetic properties was investigated. As-deposited nickel ferrite thin films were cubic in crystal structure. Calculated grain size after annealing was increased from 30 to 48 nm in addition to formation of rough surface morphology. Due to decrease in defect levels after air baking the annealed nickel ferrite thin film showed saturation magnetization of 268 emu/cc, higher than non-annealed (230 emu/cc), when used in magnetic studies.     

Relationship between distortion of crystal structure and dielectric properties of complex perovskite oxide Ba(Co,Zn)1/3Nb2/3O3 thin films

The oxygen octahedral can be distorted by epitaxial strain due to the lattice mismatch. The epitaxial strain (ε_yy) linearly decreases from ? 0.244% to ? 0.445% with the growth temperature. Thin films grow along c axis on the SrTiO₃ substrate and exhibit the epitaxial relationship of Ba(Co,Zn)_1/3Nb_2/3O₃ (001) // SrTiO₃ (001). The superlattice reflections arising from in-phase tilting of the oxygen octahedra are clearly visible along [010] and [111] zone axis. The IR modes at 330 cm^?1 and 390 cm^?1 related to in-phase tilting are observed in far-infrared reflectivity spectroscopy. The calculated Q×f values from far-infrared reflectivity spectra of films grown at 550 °C to 700 °C increases from 51,000 GHz to 91,000 GHz mainly due to the enhancement of crystalline quality. The intrinsic quality factor (Q) is mainly contributed by O-(Co, Nb)-O and O-(Zn, Nb)-O bonding modes, while in-phase tilting in BCZN films may result in enhanced dielectric constants.     

Influence of WS2 content on high temperature wear performance of magnetron sputtered TiN-WSx thin films

TiN-WS_x thin films with varying WS_x content were co-deposited by reactive magnetron sputtering. GAXRD analyses showed that the addition of 4 at.% WS_x led to loss of crystallinity of TiN phase and a complete amorphous characteristic was manifested upon incorporation of 19 at.% WS_x. Nanohardness results indicated that TiN-WS_x containing 4 and 19 at.% WS_x presented 19.7 GPa and 18.4 GPa, respectively, following the rule of mixtures. Friction coefficient and wear rates measured in reciprocated tribological tests revealed that TiN-WS_x coatings present an improved tribological performance when compared to pure TiN thin film at room temperature, registering friction coefficient of 0.42 ± 0.05 and 0.19 ± 0.03 for samples with 4 and 19 at.% WS_x, respectively. Wear tests at high temperatures evidenced that sample with 4 at.% WS_x did not provide advanced protection to substrate at 343 K and above due to deterioration. On the other hand, coating with 19 at.% WS_x maintained low friction coefficient up to 343 K, registering an optimum wear rate of 0.86 × 10⁻¹⁷ m²/N with no cracking occurrence.     

Phase transformation and growth mechanism of RF sputtered ferroelectric lead scandium tantalate (PbSc0.5Ta0.5O3) films

Lead scandium tantalate (PbSc_0.5Ta_0.5O₃, PST), an order/disorder ferroelectric, is a potential candidate for electrocaloric cooling and pyroelectric infrared (IR) detector. In this work, we report the phase transformation kinetics from two series of samples containing pure amorphous and mixture of amorphous and pyrochlore to desired perovskite phase using postdeposition rapid thermal processing (RTP) as well as growth mechanism of RF sputtered PST thin films using excess lead target on platinized silicon (Pt/Ti/SiO₂/Si) substrates. We find that small changes in the temperature ramp have a large effect on the degree of perovskite conversion (ferroelectric phase), orientation (crystallographic texture), and long-range order parameter (< S₁₁₁ >). Through isothermal annealing, we obtained optimal perovskite phase at ≥700°C temperature. The phase transformation is characterized by spontaneous formation of center-type in-plane radial rosette-like structures revealed by scanning electron microscopy. The PST perovskite crystallites were found to coexist with pyrochlore in RTP annealed films. The volume fractions for perovskite and pyrochlore phase were obtained from the analysis of “rosettes” and respective X-ray diffraction intensities which helped to determine various parameters associated with phase kinetics (n, k, and activation energy, E_a) and accompanying growth. The effective activation energies of perovskite transition and growth were found to be 332 ± 11 kJ/mol (345 ± 11 kJ/mol) and 114 ± 10 kJ/mol (122 ± 10 kJ/mol), respectively, for pure amorphous only (and mixed amorphous and pyrochlore) phase following nucleation-growth controlled Avrami's equation. A linear growth rate (n∼1) for the perovskite phase indicates predominant interface-controlled process and diffusion-limited phenomena thus inhibiting rosette size owing to reactant depletion and soft impingement at the grain boundary. However, the growth behavior is isotropic in two-dimension parallel to the plane of the substrates for both sample series. Lead loss was severe for in-situ growth and RTP combined with conventional furnace annealing than those of RTP only films, which were closer to stoichiometric albeit with excess lead and marginal oxygen vacancies (V_o).     

Structural and thermal studies of silver nanoparticles and electrical transport study of their thin films

This work reports the preparation and characterization of silver nanoparticles synthesized through wet chemical solution method and of silver films deposited by dip-coating method. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), field emission transmission electron microscopy (FETEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), and energy dispersive spectroscopy (EDX) have been used to characterize the prepared silver nanoparticles and thin film. The morphology and crystal structure of silver nanoparticles have been determined by FESEM, HRTEM, and FETEM. The average grain size of silver nanoparticles is found to be 17.5 nm. The peaks in XRD pattern are in good agreement with that of face-centered-cubic form of metallic silver. TGA/DTA results confirmed the weight loss and the exothermic reaction due to desorption of chemisorbed water. The temperature dependence of resistivity of silver thin film, determined in the temperature range of 100-300 K, exhibit semiconducting behavior of the sample. The sample shows the activated variable range hopping in the localized states near the Fermi level.     

Effect of sputtering power on piezoresistivity and interfacial strength of SiCN thin films prepared by magnetic sputtering

SiCN ceramics show large potential in high temperature pressure sensors with excellent stability up to 1000 °C, as it is changeling for the most of the existing pressure sensors to work stably at a temperature above 600 °C. However, bulk SiCN ceramics are not compatible to microelectronic processing and exhibit slow response due to viscoelasticity, it is necessary to propose alternative method to prepare SiCN functional structures. In this work, SiCN piezoresistive thin films are prepared by magnetron sputtering, and the influence of sputtering power on their piezoresistive properties and interfacial strengths are studied. The gauge factors of SiCN films range from 2786 to 4714 at various sputtering powers, which are significantly higher than the range from 46 to 1105 for existing piezoresistive thin films. Upon an optimal sputtering power of 75 W for silicon nitride target, the obtained SiCN sample show the largest gauge factors in a large range from 0.5 to 3.4 MPa. Furthermore, the SiCN thin films present high critical loads up to 36.5 N in scratch tests and indicate strong interfacial adhesion with substrate. This work provides an important reference for developing SiCN-based MEMS pressure sensors.     

Effects of annealing atmospheres on the structure and ferromagnetic properties of Fe0.12Cu0.02Zn0.86O thin films

Fe_0.12Cu_0.02Zn_0.86O thin film was deposited on a Si substrate using r. f. sputtering with no heating and an Ar/O₂ ratio of 10%. After deposition, the specimens were annealed at 400 °C for 1 h, in nitrogen and hydrogen atmospheres. The X-ray diffractometry (XRD) analysis results show that the crystallinity of Fe_0.12Cu_0.02Zn_0.86O thin film annealed in a nitrogen atmosphere is better than that of the film annealed in a hydrogen atmosphere. The X-ray photoelectron spectroscope (XPS) results show that there are more oxygen vacancies in the Fe_0.12Cu_0.02Zn_0.86O thin film annealed in a hydrogen atmosphere. The magnetic force microscope (MFM) analysis results also demonstrate that some magnetism particles are precipitated for the Fe_0.12Cu_0.02Zn_0.86O thin film annealed in a hydrogen atmosphere. This results in an improvement in the ferromagnetic properties, and the saturation magnetization is 70.2 emu/cm³, which is about 25% larger than that for the as-grown Fe_0.12Cu_0.02Zn_0.86O thin film.     

High‐performance varistors prepared by hot‐dipping tin oxide thin films in Sb2O3 powder: Influence of temperature

A series of SnO_x–Sb₂O₃ thin film varistors were fabricated through hot‐dipping tin oxide films deposited by radio‐frequency magnetron sputtering in Sb₂O₃ powder at varied temperatures in air. With the increase in hot‐dipping temperature (HDT) from 200°C to 600°C, the nonlinear coefficient (α) of the samples increased first and then decreased, reaching the maximum at 500°C, which was mainly determined by the completeness of high‐resistant Sb₂O₃ layer at tin oxide grain boundary and the chemical composition of tin oxide films. Correspondingly, the leakage current (I_L) decreased first and increased later. The breakdown electric field (E_100 mA) decreased constantly with increasing HDT. The SnO_x–Sb₂O₃ film varistors prepared at 500°C exhibited the optimum nonlinear properties with the maximum α of 10.88, the minimum I_L of 36.3 mA/cm², and an E_100mA of 0.0188 V/nm. The obtained nanoscaled film varistors would be promising in electrical/electronic devices working in low voltage.     

Tunable structural transition and multiferroic properties of the composite thin films through the structural transition of magnetic layer

The Bi_0.9Er_0.1Fe_0.96Mn_0.02Co_0.02O₃/Co_1-xMn_xFe₂O₄ (BEFMCO/CM_xFO) thin films have been deposited by sol-gel method. Structural distortion is observed in the BEFMCO with the appearance of trigonal-R-3m: H in the CM_xFO. The enhanced multiferroic properties, well electrically writable and ferroelectric switching properties are obtained in BEFMCO/CM_xFO thin films. The investigation indicates that the structural transformation of the CM_xFO influences the structure and multiferroic properties of BEFMCO and the interfacial effects between BEFMCO and CM_xFO layers. This transformation and Mn-doping cause the change of carriers, which solves the problem that the magnetic layer exacerbates the ferroelectric properties. It promotes to form the weak local electric field, which causes the weak interface effect, and brings out the weak resistive switching in the BEFMCO/CM_xFO thin films. Therefore, it is believed that the BEFMCO/CM_xFO films can offer a potentially tunable structural transformation of composite films for practical applications.     

Fabrication of Pb(Zr,Ti)O3 thin films utilizing unconventional powder magnetron sputtering (PMS)

Pb(Zr,Ti)O3 (PZT) ferroelectric ceramic films exhibit highly superior ferroelectric, pyroelectric and piezoelectric properties which are promising for a number of applications including non-volatile random access memory devices, non-linear optics, motion and thermal sensors, tunable microwave systems and in energy harvesting (EH) use. In this research, a thin layer of PZT was deposited on two different substrates of Strontium Titanate (STO) and Strontium ruthenate (SRO) by powder magnetron sputtering (PMS) system. The preliminary powders, consisting of PbO, ZrO₂ and TiO_2, were manually mixed and placed into the target holder of the PMS. The deposition was performed at an elevated temperature reaching up to 600 °C via a ceramic heater. This high temperature is required for PZT thin film crystallinity, which is never achieved in conventional physical vapour deposition processes. The phase structure, crystallite size, stress-strain and surface morphology of deposited thin films were characterized using X-ray Diffraction (XRD) and Field Emission Scanning Electron Microscopy (FESEM). The composition of the PZT thin films were also analysed by X-ray photoelectron spectroscopy (XPS). The mechanical properties of the thin films were evaluated with micro-scratch adhesive strength and micro hardness equipment. FESEM results showed that the PZT thin films were successfully deposited on both SRO and STO substrates. The surfaces of the coated samples were free from cracks, relatively smooth, uniform and dense. The profile of X-ray diffraction confirmed the formation of single-c-domain/single crystal perovskite phase grown on both substrates. The XPS analysis have shown that the PZT thin film grown by this method and that a target of PZT+10% PbO is a proper target for growing nominal PZT thin films. The adhesion strength and micro hardness results have confirmed the stability and durability of the thin film on the substrates, although higher values have been reported for thin film of PZT deposited on SRO surfaces.