Conducting and topographic AFM analysis of Hf-doped and Al-doped Ta2O5 films

A conductive atomic force microscopy (C-AFM) has been used to study conductivity and electrical degradation of ultrathin (4 nm) Hf- and Al-doped Ta₂O₅ at the nanometer scale. The hardness testing has been also performed using the force measuring ability of the AFM. Since the size of the analyzed area is very small, features which are not visible by macroscopic tests are observed: extremely low leakage current (~ pA) up to significantly higher than the fields during standard current-voltage measurements; charge trapping/detrapping processes manifesting as current peaks at pre-breakdown voltages. Hf and Al addition improves the local conductivity of Ta₂O₅, provokes modification of the leakage current mechanism, and is effective in extending the potential of pure Ta₂O₅ as a high-k material at the nanoscale. The results point to a decisive role of the type of the dopant on the electrical and mechanical properties of the films and their local response to short term microwave irradiation. Hf-doped Ta₂O₅ exhibits excellent electrical stability and high hardness. Al doping provides more plastic films with large electrical inhomogeneities; the microwave treatment at room temperature is a way to improve these parameters to a level comparable to those of Hf-doped films.     

Study and fabrication of ZnNb2O6 thin films by sol-gel method

Zinc niobium oxide (ZnNb₂O₆) thin films were grown on ITO/glass substrate by sol-gel process. Microstructure and surface morphology of the ZnNb₂O₆ thin films have been studied by X-ray diffraction and scanning electron microscopy. Optical properties of the ZnNb₂O₆ thin films were obtained by UV-visible recording spectrophotometer. The dependence of the microstructure, optical transmittance spectra, optical band gap on annealing temperature was also investigated.     

Structural and optical properties of ZnO films grown on silicon and their applications in MOS devices in conjunction with ZrO<Subscript>2</Subscript> as a gate dielectric

Photoluminescence (PL) properties of undoped ZnO thin films grown by rf magnetron sputtering on silicon substrates have been investigated. ZnO/Si substrates are characterized by Rutherford backscattering (RBS), X-ray diffraction (XRD), Fourier transform infrared (FTIR), and X-ray photoelectron spectroscopy (XPS). ZrO₂ thin films have been deposited on ZnO using microwave plasma enhanced chemical vapour deposition at a low temperature (150°C). Using metal insulator semiconductor (MIS) capacitor structures, the reliability and the leakage current characteristics of ZrO₂ films have been studied both at room and high temperatures. Schottky conduction mechanism is found to dominate the current conduction at a high temperature. Good electrical and reliability properties suggest the suitability of deposited ZrO₂ thin films as an alternative as gate dielectric on ZnO/n-Si heterostructure for future device applications.     

Gravitational waves detector mirrors: Spectroscopic ellipsometry study of Ta2O5 films on SiO2 substrates

A stack of Ta₂O₅/SiO₂ layers is presently used as coating layer of mirrors in interferometric detectors for gravitational waves. The sensitivity of these detectors is limited in the 50-300 Hz frequency range by the mirror thermal noise, and it was suggested that mechanical losses in the Ta₂O₅ are the dominant source of noise. We focus here on Spectroscopic Ellipsometry (SE) results (in the 0.75 ÷ 5 eV spectral range) obtained on high quality Ta₂O₅ films deposited on SiO₂ substrates by Double Ion Beam Sputtering at the Laboratoire des Matériaux Avancés (Lyon, France). The films are extremely flat as indicated by the 0.2 nm RMS roughness determined by Atomic Force Microscopy (AFM) on (20 × 20) μm² areas. The comparison of the optical properties determined by SE with literature data, corroborated by X-ray Photoelectron Spectroscopy (XPS) data, suggests that the films present a non-ideal bulk stoichiometry and/or some degree of nanoporosity. The possible influence of an interface layer is also discussed.     

Phase developments in the Pb(Zn1/2W1/2)O3-Pb(Zn1/3Ta2/3)O3-Pb(Zn1/3Nb2/3)O3 pseudo-ternary system

The phase stability ranges in the B-site precursor (Zn_1/2W_1/2)O₂-(Zn_1/3Ta_2/3)O₂-(Zn_1/3Nb_2/3)O₂ were determined by X-ray diffraction (XRD), where wolframite, tri-αPbO₂, and columbite phases were identified. Next attempts were carried out (with the addition of PbO) for the system Pb(Zn_1/2W_1/2)O₃-Pb(Zn_1/3Ta_2/3)O₃-Pb(Zn_1/3Nb_2/3)O₃, where the perovskite phase did not develop in the entire compositions investigated. Instead, only the Pb₂WO₅ and pyrochlore phases (along with ZnO) resulted.     

Nanometer sized tantalum pentoxide fibers prepared by electrospinning

Novel, porous tantalum pentoxide (Ta₂O₅) nanofibers with 150–250 nm diameter were obtained by high temperature calcination of the as-electrospun tantalum pentoxide/poly(vinyl acetate) (PVAc) composite fibers prepared by sol–gel processing and electrospinning technique. Surface analysis, structure and elemental composition of these as-electrospun and as-calcinated Ta₂O₅ nanofibers have been studied by scanning electron microscope (SEM) equipped with an energy dispersive X-ray analysis (EDX), high resolution field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray diffraction patterns (XRD) and FT-IR. High-resolution FE-SEM images showed the porous nature of Ta₂O₅ nanofibers. EDX analysis revealed the perfect stoichiometry of the nanofibers as Ta₂O₅. A linear correlation was noted between the calcination temperature and orthorhombic crystalline phase evolution of Ta₂O₅.     

Electrical characteristics of Ti-O/Ta2O5 thin film sputtered on Ta/Ti/Al2O3 substrate

The electrical characteristics of Ti-O/Ta₂O₅ films sputtered on Ta/Ti/Al₂O₃ substrate were investigated. Ta (tantalum) was used for the bottom and upper electrodes for the purpose of simplifying the fabrication process and Al₂O₃ substrates were used, which are needed in integral passive devices. Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors were annealed at 700 °C for 60 s in vacuum. The X-ray diffraction pattern (XRD) results showed that as-deposited Ta had a highly preferred orientation, but Ta₂O₅ film had amorphous structure, which was transformed to crystallization structure by rapid thermal heat treatment. We examined the log J-E and C-V characteristics of the dielectric thin films deposited on the Ta bottom electrode. From these results, we concluded that the leakage current could be reduced by introducing a Ti-O buffer layer. The conduction mechanisms of Ta/Ti-O/Ta₂O₅/Ta/Ti/Al₂O₃ capacitors could be interpreted appropriately by hopping conduction in lower field (E<1×10⁵ V/cm) and space-charge-limited current in higher fields (1×10⁵ V/cm<E).     

Structural and electrical properties of Ta<Subscript><Emphasis Type="Bold">2</Emphasis></Subscript>O<Subscript><Emphasis Type="Bold">5</Emphasis></Subscript> thin films prepared by photo-induced CVD

Tantalum oxide (Ta ₂ O ₅ ) films and Al/Ta ₂ O ₅ /Si MOS capacitors were prepared at various powers by ultraviolet photo-inducing hot filament chemical vapour deposition (HFCVD). Effects of ultraviolet light powers on the structure and electrical properties of Ta ₂ O ₅ thin films were studied using X-ray diffraction (XRD) and atomic force microscopy (AFM). The dielectric constant, leakage current density and breakdown electric field of the samples were studied by the capacitance–voltage (C–V) and current–voltage (I–V) measurements of the Al/Ta ₂ O ₅ /Si MOS capacitors. Results show that the Ta ₂ O ₅ thin films grown without inducement of UV light belong to amorphous phase, whereas the samples grown with inducement of UV-light belong to δ-Ta ₂ O ₅ phase. The dielectric constant and leakage current density of the Ta ₂ O ₅ thin films increase with increasing powers of the UV- lamps. Effects of UV- lamp powers on the structural and electrical properties were discussed.     

Composition and Morphology of Electrodeposited CuInSe2 Precursor Films

CuInSe₂ (CIS) precursor films have been prepared by electrodeposition in aqueous solution. The electrodeposited films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) for structural, morphological and componential properties. The influence of deposition potential and Na-citrate concentration on composition and morphology of electrodeposited films was studied in detail. It is found that the film morphology is strongly influenced by deposition potential and Na-citrate concentration. Films with large and homogenous grain size and ratio of Cu/In approaching 1 were obtained at deposition potentials of -0.7 and -0.75 V vs the saturated calomel electrode (SCE) and Na-citrate concentration of 500 mmol/L. Chalcopyrite phase CuInSe₂ is contained in precursor films that have poor crystallinity.     

Residual stress of graded-index-like films deposited by radio frequency ion-beam sputtering

In this study, Ta₂O₅-SiO₂ composite films with various proportions of Ta₂O₅ were prepared by radio frequency ion-beam sputtering deposition. The residual stress of each composite film was analyzed. The residual stresses of different graded-index-like layers made of composite films were studied. The results show that the residual stress of a single layered composite film was lower than that of pure SiO₂ or a pure Ta₂O₅ film. Furthermore, when the composite film was made graded-index-like, the residual stress was reduced.     

The effects of O2/Ar ratio on the structure and properties of hafnium dioxide (HfO2) films

HfO₂ films at various O₂/Ar flow ratios were prepared by reactive dc magnetron sputtering. The effects of O₂/Ar ratio on the structure and properties of HfO₂ films were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and UV-Visible spectroscopy. The results showed that the HfO₂ films were amorphous at different O₂/Ar ratios, and the atomic ratio of O/Hf in the HfO₂ films at high O₂/Ar ratio was nearly to 2:1. The peaks of Hf4f and O1s shifted to higher binding energy with increasing the oxygen flow proportion. The HfO₂ films at high O₂/Ar ratio had high transmissivity at the range of 400-1100 nm.     

Influence of oxygen pressure on the structural, electrical and optical properties of VO2 thin films deposited on ZnO/glass substrates by pulsed laser deposition

The influence of oxygen pressure on the structural and electrical properties of vanadium oxide thin films deposited on glass substrates by pulsed laser deposition, via a 5-nm thick ZnO buffer, was investigated. For the purposes of comparison, VO₂ thin films were also deposited on c-cut sapphire and glass substrates. During laser ablation of the V metal target, the oxygen pressure was varied between 1.33 and 6.67 Pa at 500 °C, and the interaction and reaction of the VO₂ and the ZnO buffer were studied. X-ray diffraction studies showed that the VO₂ thin film deposited on a c-axis oriented ZnO buffer layer under 1.33 Pa oxygen had (020) preferential orientation. However, VO₂ thin films deposited under 5.33 and 6.67 Pa were randomly oriented and showed (011) peaks. Crystalline orientation controlled VO₂ thin films were prepared without such expensive single crystal substrates as c-cut sapphire. The metal-insulator transition properties of the VO₂/ZnO/glass samples were investigated in terms of electrical conductivity and infrared reflectance with varying temperatures, and the surface composition was investigated by X-ray photoelectron spectroscopy.     

Effects of annealing in O2 and N2 on the microstructure of metal organic chemical vapor deposition Ta2O5 film and the interfacial SiO2 layer

Ta₂O₅ films were made by metal organic chemical vapor deposition (MOCVD) and annealed at various temperatures under N₂ and O₂ ambients in a conventional furnace and a rapid thermal reactor (RTR). The microstructure and composition of the Ta₂O₅ film and the interfacial SiO₂ layer before and after various annealing treatments were studied using X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and Auger electron spectroscopy (AES). The as-deposited Ta₂O₅ film has an amorphous structure. The surface topology of the as-deposited Ta₂O₅ film is smooth without any apparent features. Annealing of the as-deposited film results in crystallization to an orthorhombic structure with (1 0 0) preferred orientation, and an increase in surface roughness, with the appearance of grain boundaries under AFM. The crystallization temperature varies in the various annealing treatments. An interfacial SiO₂ layer was found between the as-deposited/annealed Ta₂O₅ films and silicon substrate. The annealing treatments result in an increase in thickness of the SiO₂ layer and roughness changes of the Ta₂O₅/SiO₂/Si interfaces, which are discussed in terms of element diffusion and thermodynamic stability.     

Efficient and green oxidative degradation of methylene blue using Mn-doped ZnO nanoparticles (Zn1−xMnxO)

Mn-doped ZnO nanoparticles, Zn_1?xMn_xO, were synthesised by a polyethylene glycol (PEG) sol–gel method and the physicochemical properties of compounds were characterised by atomic absorption spectroscopy (AAS), energy-dispersive X-ray analysis, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The catalytic degradation of an organic dye, methylene blue (MB), in the presence of Zn_1?xMn_xO as the catalyst and hydrogen peroxide (H₂O₂) as the oxidant at room temperature in water has been studied. Effects of oxidant, catalyst amount, catalyst composition, pH value of the solution and an OH-radical scavenging agent on the degree of the decomposition of MB dye were also studied.     

Synthesis of K6Ta10.8O30 nanowires by molten salt technique

The synthesis of single crystalline K₆Ta_10.8O₃₀ nanowires by molten salt method was reported for the first time. X-ray diffraction results indicated that the as-prepared products were pure phase K₆Ta_10.8O₃₀. Scanning electron microscopy and transmission electron microscopy results showed that the products consisted of wire-like nanostructures with 100-300 nm in diameter and several micrometers in length. High resolution electron microscopy and selected area electron diffraction results indicated that the K₆Ta_10.8O₃₀ nanowires were single crystalline with a growth direction of [0 0 1]. The ultraviolet-visible diffuse reflectance measurement showed that the band gap of the nanowires was about 4.1 eV. The effects of reaction temperature, time, and weight ratio of the precursor (mixture of K₂CO₃ and Ta₂O₅) to KCl salt on the morphology of the products were investigated.     

Properties of (K,Na)NbO3-based lead-free piezoelectric films prepared by pulsed laser deposition

To investigate the properties of (K,Na)NbO₃-based lead-free piezoelectric films at the morphotropic phase boundary composition, we fabricated epitaxial [(K_0.5Na_0.5)_0.97Li_0.03] (Nb_0.8Ta_0.2)O₃ films on (001), (110) and (111)-oriented single crystal SrTiO₃ substrates by pulsed laser deposition. The structure and electrical properties of the films were studied. Dielectric constants of 540, 390 and 300 and remnant polarizations of 4.00, 1.05, and 0.35 μC/cm² were observed for the (001), (110) and (111) oriented films, respectively.     

Characterization of high quality tantalum pentoxide film synthesized by oxygen plasma enhanced pulsed laser deposition

Tantalum pentoxide films were deposited on BK7 glass substrates using oxygen plasma enhanced pulsed laser deposition (OPE-PLD). X-ray diffraction, atomic force microscopy, ultraviolet–visible–near infrared scanning spectrophotometry, and spectroscopic ellipsometry were used to characterize the crystallinity, microscopic morphology and optical properties of films. Results show that the film roughness increased with the increase of oxygen pressure, and decreased with the application of OPE. Meanwhile the use of oxygen plasma in a 2 Pa O₂ pressure resulted in the transmittance of the thin film of 91.8% at its peak position (the transmittance of bare substrate). Moreover, the root-mean-square roughness as low as 0.736 nm, and refractive index of 2.18 at 633 nm wavelength, close to the refractive index of bulk Ta₂O₅ (~ 2.20 at 633 nm wavelength), were obtained.     

Synthesis and properties of β-Ga2O3 nanostructures

A novel method was utilized to synthesize one-dimensional β-Ga₂O₃ nanostructures. In this method, β-Ga₂O₃ nanostructures have been successfully synthesized on Si(111) substrates through annealing sputtered Ga₂O₃/Mo films under flowing ammonia in a quartz tube. The as-obtained samples were analyzed in detail using the methods of X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDX) attached to the HRTEM instrument. The results show that the formed nanostructures are single-crystalline Ga₂O₃. The annealing temperature has an evident influence on the morphology of the β-Ga₂O₃ nanostructures. The growth mechanism of the β-Ga₂O₃ nanostructures is also discussed by conventional vapor-solid (VS) mechanism.     

Fabrication of KTa0.65Nb0.35O3 film by pulsed laser deposition on glass substrate with various buffer layers

KTa_0.65Nb_0.35O₃ (KTN) thin films were deposited on amorphous glass substrates using a range of single buffer layers such as indium tin oxide (ITO), zinc oxide (ZnO), 3 at% Al-doped ZnO (AZO), and 3 at% Ga-doped ZnO (GZO), as well as a variety of multi-buffer layers such as SrTiO₃ (STO)/ITO, STO/ZnO, STO/AZO, and STO/GZO using a pulsed laser deposition system. All films showed a polycrystalline perovskite phase with the exception of all single buffer layers and STO/ITO multi-buffer layers. The STO buffer layer is important for crystallizing KTN films due to the similar lattice constant and same crystal structure. The optical transmittance of all films exhibited a transmittance ?90% in the wavelength range.     

The effect of Sb2O5 additions on the dielectric properties of Ag(Nb0.8Ta0.2)O3 ceramics

The sintering behavior and dielectric properties for perovskite Ag(Nb_0.8Ta_0.2)O₃ ceramic with Sb₂O₅ doping was explored. A small amount of Sb₂O₅ (2.5 wt.%) led to high densification at temperatures < 1060 °C. The dielectric constant increased and the temperature coefficient decreased with increasing concentration of Sb₂O₅, and the dielectric constant reached 673, combined with a low temperature coefficient of 147 ppm/°C, and dielectric loss of 0.0044 (at 1 MHz) for the sample with 3.5 wt.% Sb₂O₅ sintered at 1080 °C.