Synthesis of two-dimensional gallium nitride via spin coating method: influences of nitridation temperatures

This paper reports the synthesis and characterization of gallium nitride (GaN) thin films deposited on p-type silicon (100) substrates by using low cost spin coating method under various nitridation temperatures. This work demonstrated that spin coating with the new prepared precursor solution can be used as a versatile method for the successfully growth of GaN thin films. Furthermore, the influence of varying nitridation temperatures on the structural, morphological, and optical properties of synthesized GaN thin films were studied in this work. The GaN thin films were characterized by X-ray diffraction, field-emission scanning electron microscopy, atomic force microscopy, photoluminescence and Raman spectroscopy. All the characteristics of the GaN thin films were effectively improved with the increasing of the nitridation temperatures from 750 to 950 °C and degraded at temperature of 1,050 °C. The measured results show that nitridation temperature plays an important role in improving the crystalline quality of the GaN thin films and the most efficient nitridation temperature was at 950 °C.     

Characterisation and properties of magnetron sputtered nanoscale bi‐layered Ni/Ti thin films and effect of annealing

Single‐bi‐layer of Ni–Ti thin film was deposited using DC and RF magnetron sputtering technique by layer‐wise deposition of Ni and Ti on Si(100) substrate in the order of Ni as the bottom layer and Ti as the top layer. The deposition of these amorphous as‐deposited thin films was followed by annealing at 300 °C, 400 °C, 500 °C, and 600 °C temperature with 1‐h annealing time for each to achieve crystalline thin films. This paper describes the fabrication processes and the novel characterization techniques of the as‐deposited as well as the annealed thin films. Microstructures were analysed using FESEM and HRTEM. Nano‐indentation and AFM were carried out to characterize the mechanical properties and surface profiles of the films. It was found that, for the annealing temperatures of 300 °C to 600 °C, the increase in annealing temperature resulted in gradual increase in atomic‐cluster coarsening with improved ad‐atom mobility. Phase analyses, performed by GIXRD, showed the development of silicide phases and intermetallic compounds. Cross‐sectional micrographs exhibited the inter‐diffusion between the two‐layer constituents, especially at higher temperatures, which resulted either in amorphization or in crystallization after annealing at temperatures above 400 °C. Copyright © 2015 John Wiley & Sons, Ltd.     

Structure and voltage tunable dielectric properties of sol–gel derived Bi1.5MgNb1.5O7 thin films

Bi_1.5MgNb_1.5O₇ (BMN) thin films were fabricated on Au/Ti/SiO₂/Si(100) substrates using a sol?Cgel spin coating process. Thermo decomposition of the BMN precursor gel was discussed. The structures, morphologies, dielectric properties and voltage tunable dielectric properties were investigated. The deposited films showed a cubic pyrochlore structure after annealing at 550?°C or higher temperatures. With the annealing temperature increased from 500 to 800?°C, the root-mean-square surface roughness of the films increased from 0.6 to 6.8?nm. Additional phase, MgNb₂O₆, emerged after annealing at 800?°C due to the volatilization of Bi element. The dielectric properties and tunability of the films were annealing temperature dependent. BMN thin films annealed at 750?°C had a high dielectric constant of 135 and low dielectric loss of 0.002 at 1?MHz. The high tunability of 31.3?% and figure of merit of 156.5 were obtained under an applied electric field of 1?MV/cm at room temperature.     

Substrate temperature effects on the structural,compositional, and electrical properties of VO2 thin films deposited by pulsed laser deposition

The vanadium dioxide (VO₂) thin films were deposited on silicon (100) substrate using the pulsed laser deposition technique. The thin films were deposited at different substrate temperatures (500°C, 600°C, 700°C, and 800°C) while keeping all the other parameters constant. X‐ray diffraction confirmed the crystalline VO₂ (B) and VO₂ (M) phase formation at different substrate temperatures. X‐ray photoelectron spectroscopy analysis showed the presence of V⁴⁺ and V⁵⁺ charge states in all the deposited thin films which confirms that the deposited films mainly consist of VO₂ and V₂O₅. An increase in the VO₂/V₂O₅ ratio has been observed in the films deposited at higher substrate temperatures (700°C and 800°C). Scanning electron microscope micrographs revealed different surface morphologies of the thin films deposited at different substrate temperatures. The electrical properties showed the sharp semiconductor to metal transition behavior with approximately 2 orders of magnitude for the VO₂ thin film deposited at 800°C. The transition temperature for heating and cooling cycles as low as 46.2°C and 42°C, respectively, has been observed which is related to the smaller difference in the interplanar spacing between the as‐deposited thin film and the standard rutile VO₂ as well as to the lattice strain of approximately −1.2%.     

Structure and dielectric properties of HfO<Subscript>2</Subscript> films prepared by a sol–gel route

Mono- and multilayer HfO₂ sol–gel thin films have been deposited on silicon wafers by dip-coating technique using a solution based on hafnium ethoxide as precursor. The densification/crystallization process was achieved by classical annealing between 400 and 600 °C for 0.5 h (after drying at 100 °C). Systematic TEM studies were performed to observe the evolution of the thin film structure depending on the annealing temperature. The overall density of the films was determined from RBS spectrometry correlated with cross section (XTEM) thickness measurements. After annealing at 450 °C the films are amorphous with a nanoporous structure showing also some incipient crystallization. After annealing at 550 °C the films are totally crystallized. The HfO₂ grains grow in colonies having the same crystalline orientation with respect to the film plane, including faceted nanopores. During annealing a nanometric SiO₂ layer is formed at the interface with the silicon substrate; the thickness of this layer increases with the annealing temperature. Capacitive measurements allowed determining the value of the dielectric constant as 25 for four layer films, i.e. very close to the value for the bulk material.     

Effect of Annealing on the Electrical Properties of CuxS Thin Films

Copper sulphide CuS was deposited on three substrates; glass, Indium Tin Oxide (ITO) and Ti by using spray pyrolysis deposition (SPD). After depositing CuS thin films on the substrates at 200 °C, they were annealed at 50, 100, 150, and 200 °C for 1 hour. Structural measurements revealed covellite CuS and chalcocite Cu₂S phases for thin films before and after annealing at 200 °C with changes in intensities, and only covellite CuS phase for thin films after annealing at 50, 100, and 150 °C. Morphological characteristics show hexagonal-cubic crystals for the CuS thin film deposited on glass substrate and plates structures for films deposited on ITO and Ti substrates before annealing, these crystals became bigger in size and there were be oxidation and some agglomerations in some regions with formation of plates for CuS on glass substrate after annealing at 200 °C. For Hall Effect measurements, thin films sheet resistivity and mobility increased after annealing while the carrier concentration decreased. Generally, the thin film deposited on ITO substrate had the lowest resistivity and the highest carrier concentration before and after annealing. The thin film deposited on Ti substrate had the highest mobility before and after annealing, which makes it the best thin film for device performance. The objective of this research is to show the improvement of thin films electrical properties especially the mobility after annealing those thin films.     

Effect of post‐deposition annealing on surface morphology and gas sensing properties of palladium phthalocyanine thin films

The effect of post‐deposition annealing on surface morphology and gas sensing properties of palladium phthalocyanine (PdPc) nanostructured thin films has been studied. PdPc thin films were deposited on polyborosilicate substrate by thermal evaporation technique at room temperature. The surface morphology of thin films was investigated by SEM, X‐ray diffraction, and optical absorption. X‐ray diffraction patterns showed a phase transition from α to β based on post‐deposition annealing at temperatures above 200 °C. The SEM and optical absorption confirmed that annealing strongly influenced the surface morphology of nanostructured thin films. Sandwich devices (Au|PdPc|Al) were fabricated and exposed to different concentrations of NO₂ and NH₃ as oxidizing and reducing gases at different temperatures, and the sensitivity of devices were obtained versus gases. Obtained results showed α‐PdPc thin film devices had higher sensitivity in comparison with devices in β‐phase. In particular, it was found that the sensitivity of devices is temperature dependent and the best operating temperature range of devices was measured at about 90–100 °C. Devices showed good reversibility, response, and recovery time at room temperature. Finally, the stability of sensors was investigated for a period of about 1 year; results showed that the sensors were stable for 2 months and lost about 30% of their sensitivity after 1 year. Copyright © 2012 John Wiley & Sons, Ltd.     

Preparation of ordered mesoporous TiO2 thin film and its application in methanol catalytic combustion

Ordered mesoporous titania thin films were synthesized by evaporation induced self‐assembly process in the presence of Pluronic block copolymers P123 (EO₂₀‐PO₇₀‐EO₂₀). The influence of several experimental parameters, including aging humidity, aging temperature, substrate properties and methods for organic templates removal, on the mesostructure of titania thin films was investigated in details. The mesoporous titania thin film supported Pt catalyst was prepared, and its methanol catalytic combustion performance was studied. The results showed that mesoporous titania thin film is an active support for catalyst. Mesoporous titania thin film supported platinum catalysts yields 70% methanol conversion at room temperature and 100% conversion at 100 °C. Copyright © 2013 John Wiley & Sons, Ltd.     

Effects of deposition temperature and annealing temperature on the morphology and electrochemical capacitance of Ni(OH)2 thin films

In this paper, we report 3D nickel (II) hydroxide thin films with porous nanostructures prepared on Ni foam by direct current electrodeposition from aqueous solution of Ni(NO₃)₂ through basic chemicals. The effect of deposition temperature on Ni(OH)₂ thin film morphology is examined by field emission scanning electron microscopy, which is found to have significant influence on capacitance performance of Ni(OH)₂ thin films. Moreover, the effect of annealing temperature on electrochemical capacitance and long-time stability of Ni(OH)₂ thin films is investigated. An optimum-specific capacitance value of 2,447?farads?g^?1 is obtained for Ni(OH)₂ thin film deposited at 20?°C and annealed at 100?°C.     

Effect of adhesive and cohesive strength on the tribological behaviour of non‐reactively sputtered TiC thin films

Titanium carbide (TiC) thin films were deposited on D9 steel substrates at room temperature (RT), 200 °C and 400 °C. A compound TiC target was sputtered to deposit films in a non‐reactive argon atmosphere. As‐deposited films were characterised for structural, chemical and mechanical properties. Nanoindentation and scratch tests were performed to evaluate the cohesive and adhesive strength of the films, respectively. Tribological properties of the films were investigated using a tribometer. An increase in nano‐hardness from 7.2 to 10.5 GPa was observed as deposition temperature was increased. The films deposited at RT and 200 °C showed poor adhesion leading to the inferior tribological performance. In contrast, films deposited at 400 °C showed better adhesion which improved the wear resistance. Tribological behaviour of TiC thin films was correlated with contact deformation modes of coatings. These modes revealed significant role of adhesive and cohesive strength associated with the coatings. Copyright © 2009 John Wiley & Sons, Ltd.     

Effect of co-sintering temperature on the performance of SOFC with YSZ electrolyte thin films fabricated by dip-coating method

Anode-supported yttria-stabilized zirconia (YSZ) electrolyte thin films were fabricated by the dip-coating method using the simple methylethylketone/ethanol-based YSZ suspension. Influences of the sintering temperature on the performance of solid oxide fuel cells were studied. Fully dense YSZ electrolyte thin films were obtained after being sintered at 1,300 °C as well as at 1,400 or 1,500 °C through SEM observation. The open circuit voltages of the cells all reached above 1.10 V at the testing temperatures. The testing results proved that both the anode performance and the electrolyte conductivity sintered at 1,300 °C were superior to those sintered at 1,400 or 1,500 °C. Investigation on the cell voltage drop under operation condition revealed, that the sintering temperature has more significant effect on the performance of the electrodes than on the electrolyte.     

Effects of gold‐induced crystallization process on the structural and electrical properties of germanium thin films

Gold‐induced (Au‐) crystallization of amorphous germanium (α‐Ge) thin films was investigated by depositing Ge on aluminum‐doped zinc oxide and glass substrates through electron beam evaporation at room temperature. The influence of the postannealing temperatures on the structural properties of the Ge thin films was investigated by employing Raman spectra, X‐ray diffraction, and scanning electron microscopy. The Raman and X‐ray diffraction results indicated that the Au‐induced crystallization of the Ge films yielded crystallization at temperature as low as 300°C for 1 hour. The amount of crystallization fraction and the film quality were improved with increasing the postannealing temperatures. The scanning electron microscopy images show that Au clusters are found on the front surface of the Ge films after the films were annealed at 500°C for 1 hour. This suggests that Au atoms move toward the surface of Ge film during annealing. The effects of annealing temperatures on the electrical conductivity of Ge films were investigated through current‐voltage measurements. The room temperature conductivity was estimated as 0.54 and 0.73 Scm⁻¹ for annealed samples grown on aluminum‐doped zinc oxide and glass substrates, respectively. These findings could be very useful to realize inexpensive Ge‐based electronic and photovoltaic applications.     

Tuning hydrophobicity of a fluorinated terpolymer in differently assembled thin films

In the current report, casting from good solvent (acetone) and casting from mixed solvent and nonsolvent were employed for preparing thin films of terpolymer of T etrafluoroethylene (TFE), H exafluoropropylene (HFP), and V inylidene fluoride (VDF) (THV), on silicon wafers. These films revealed various morphologies and wetting behaviors depending on the solution concentration, temperature, and thin film preparation method. The THV thin films prepared by casting from good solvent showed smooth morphology with holes. The thin film prepared from a 3 wt % THV/acetone solution by casting from good solvent at 15 °C demonstrated spheres in addition to the smooth morphology, while the thin film prepared from a 5 wt % THV/acetone solution at 15 °C by casting from good solvent had a mesh‐like structure with some linked spheres. Casting the thin films from mixed solvent and nonsolvent resulted in various morphologies such as different sphere sizes embedded in a dense film layer, and hexagonal close packed structures. The thin films prepared by casting from good solvent showed a slightly hydrophobic character, with a measured water contact angle of approximately 99°, while the nonsolvent cast films had a water contact angle as high as 145°. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2017 , 55, 643–657     

Collapse transition in thin films of poly(methoxydiethylenglycol acrylate)

The thermal behavior of poly(methoxydiethylenglycol acrylate) (PMDEGA) is studied in thin hydrogel films on solid supports and is compared with the behavior in aqueous solution. The PMDEGA hydrogel film thickness is varied from 2 to 422?nm. Initially, these films are homogenous, as measured with optical microscopy, atomic force microscopy, X-ray reflectivity, and grazing-incidence small-angle X-ray scattering (GISAXS). However, they tend to de-wet when stored under ambient conditions. Along the surface normal, no long-ranged correlations between substrate and film surface are detected with GISAXS, due to the high mobility of the polymer at room temperature. The swelling of the hydrogel films as a function of the water vapor pressure and the temperature are probed for saturated water vapor pressures between 2,380 and 3,170?Pa. While the swelling capability is found to increase with water vapor pressure, swelling in dependence on the temperature revealed a collapse phase transition of a lower critical solution temperature type. The transition temperature decreases from 40.6?°C to 36.6?°C with increasing film thickness, but is independent of the thickness for very thin films below a thickness of 40?nm. The observed transition temperature range compares well with the cloud points observed in dilute (0.1?wt.%) and semi-dilute (5?wt.%) solution which decrease from 45?°C to 39?°C with increasing concentration.     

Deposition of Silicon Carbide Thin Films from 1,1-Dimethyl-1-Silacyclobutane

1,1-Dimethyl-1-silacyclobutane was used as a single-source precursor to deposit SiC thin films on Si(100) and Si(111) by low-pressure chemical vapor deposition (LPCVD). Polycrystalline β-SiC thin films were grown at temperatures 1100 and 1200°C. At temperatures between 950 and 1100°C, amorphous thin films of silicon carbide were obtained. The films were studied by X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and electron diffraction (ED).     

Spectroscopic analysis of electrically polarized polyacrylonitrile

Electrically polarized and unpolarized films of polyacrylonitrile (PAN) have been investigated by both infrared attenuated total reflection (ATR) and thermally stimulated discharge (TSD). ATR analysis of PAN films has been aimed at explaining the molecular origin of thermally stimulated currents, and consequently that of phenomena contributing to electrical polarization in this material. Preferred orientation of nitrile dipoles along the thickness direction (applied electric field direction) has been detected by ATR in both polarized and unpolarized films. It is suggested that dipolar alignment in unpolarized solvent-cast films could result from internal electric fields associated with space charges. The observed orientational anisotropy is found to disappear gradually as films (both polarized and unpolarized) are heated from ambient temperature to 100°C and rotational motion in the backbone is thermally activated. TSD currents observed in this thermal range are thus associated with randomization of molecular dipoles. TSD currents observed above 100°C are suggested to originate from drift of space charges, since both an isotropic orientation of dipoles and onset of considerable diffusion are detected by ATR in this temperature range. PAN films polarized by high-intensity electric fields (5 × 10⁵Vcm^?1, as opposed to 5 × 10⁴Vcm^?1) are found to retain orientational anisotropy above 100°C, and this is believed to be associated with a structural rearrangement induced by electrical polarization.     

The influence of titanium dioxide phase composition on dyes photocatalysis

A comparative study of TiO₂ powders prepared by sol–gel methods is presented. Titanium tetraisopropoxide was used as the precursor for the sol–gel processes. The effects of the annealing treatment on phase, crystallite size, porosity and photodegradation of dyes (methyl orange and methylene blue) were studied. The phase structure, microstructure and surface properties of the films were characterized by using X-ray diffraction (XRD) and Atomic Force Microscopy (AFM). The X-ray diffraction was used for crystal phase identification, for the accurate estimation of the anatase–rutile ratio and for the crystallite size evaluation of each polymorph in the samples. It was found that the only TiO₂ anatase phase of the synthesized TiO₂ develops below 500 °C, between 600 and 800 °C the anatase coexist with rutile and above 800 °C only the rutile phase was found in the samples. Attention has been paid not only to crystal structures, but also to the porosity, the particle size and the photocatalytic properties. However, the annealing temperature was found to have significant influence on the photocatalytic properties. Different TiO₂ doctor blade thin films were obtained mixing the sol gel powder (100% anatase) and TiO₂ Aldrich with TiO₂ Degussa P25. The surfactant (Triton X100 or sodium dodecyl sulfate) affects the packing density of the particles during deposition and the photocatalytic degradation efficiency of the dyes. The photocatalytic degradation kinetics of methyl orange and methylene blue using TiO₂ thin film were investigated.     

Evolution of surface topography and optical band gap of ZnO film deposited on NiO/Si(100)

Evolution of surface features and optical band gap of ZnO thin films deposited on different NiO/Si(100) are reported. In order to create different initial microstructure, we first deposited NiO film on Si(100) at 3 different temperatures (400°C, 650°C, and 700°C) by pulsed laser deposition. These NiO/Si(100) films are used as substrate for the deposition of ZnO films. Combining the results obtained from grazing incidence X‐ray diffraction, atomic force microscope, and UV‐Visible characterization, our study indicated that the microstructure of the substrate takes the important role in dictating properties of the film. Our study also indicated that one needs to choose appropriate synthesis condition to achieve good quality ZnO films.     

Structural and electrical characterisation of betaine-type,organic, molecular,thin evaporated films and LB multilayers

The structure and electrical properties of highly polar indandione-1,3 pyridinium betaine (IPB) derivatives have been studied in vacuum-evaporated thin films and Langmuir-Blodgett (LB) multilayer assemblies. Phase transitions induced by temperature and/or electric field have been observed in LB films of an amphiphilic derivative of IPB.The LB films of IPB, obtained at room temperature, form a Y-like structure which melts at about 50 °C to produce spherical domains, having Z-like structure, which remain stable up to 110 °C. Similar phase transitions can be induced by an electric field with ε ≥ 2 × 10⁵ V cm⁻¹ at room temperature. In the new Z-like phase of the IPB LB films, the electrical conductivity increases by some five or six orders of magnitude and the activation energy of dark conductivity decreases from 0.18 ± 0.03 eV to practically zero.The vacuum-evaporated IPB films yield low electrical conductivity (σ = 10⁻¹⁵–10⁻¹⁶S cm⁻¹), whereas in the LB multilayers a notable anisotropy of conductivity is observed. In case of coplanar cells the conductivity increases to σ = 10⁻⁸S cm⁻¹. In sandwich-type LB samples the conductivity value is similar to that of the vacuum-evaporated polycrystalline thin films.     

Thermogravimetric Investigations of Nickel-Oxide Thin Films and Powders

Classical TG analysis of films supported on micro-cover glasses was performed in order to determine the appropriate processing temperature to achieve electrochemically active NiO_xH_y thin films. As deposited films made from three different precursors (Ni-acetate, nitrate and sulphate) and their corresponding powders were also investigated. From dynamic TG measurements the onset decomposition temperature could be determined. It was found out that the starting temperature of the mass change of thin films is approximately 30 degrees lower than that of the powders. A broader decomposition range was also observed for thin films. Furthermore, the isothermal treatment of films deposited on conducting substrate at 270 and 300°C was performed and by cyclic voltametry the importance of temperature and time of heating was proved. Films obtained at higher temperatures (>300°C) are electrochemically inert because of the NiO phase formation. This revised version was published online in August 2006 with corrections to the Cover Date.