Influence of bath temperatures on the wettability of copper films surface prepared by electroless plating method on beech wood

Copper films were coated on beech wood substrates by electroless plating method. The influence of bath temperature on the copper films properties was studied by varying the bath temperatures 25, 35, 45 and 55 °C. Scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS), X‐ray diffraction (XRD) pattern, X‐ray photoelectron spectroscopy (XPS), micro Raman spectroscopy and contact angle measurements were used to both characterize the physical and chemical copper films properties and understand the influence of bath temperature on the wettability of copper surface. In our studies, we have found that the gained copper mass significantly increased at 55 °C. The crystalline nature of the coated copper was confirmed by XRD. The presence of Cu₂O and CuO was observed by XPS and micro Raman techniques, which confirms the oxidization of the coated copper surface. Also these characterization techniques have shown the big influence of bath temperature on the morphology, grain size, chemical composition and the film thickness of the coated copper. The wettability was highly influenced by increasing CuO on the coated copper, which is increased by the bath temperature. The contact angle measurements have demonstrated the influence of C―O, O―C?O and CuO components of the surface on the wettability of the samples. Copyright © 2016 John Wiley & Sons, Ltd.     

Deposition of copper‐doped iron sulfide (CuxFe1−xS) thin films using aerosol‐assisted chemical vapor deposition technique

Copper‐doped iron sulfide (Cu_xFe_1?xS, x = 0.010–0.180) thin films were deposited using a single‐source precursor, Cu(LH)₂Cl₂ (LH = monoacetylferrocene thiosemicarbazone), by aerosol‐assisted chemical vapor deposition technique. The Cu‐doped FeS thin films were deposited at different substrate temperatures, i.e. 250, 300, 350, 400 and 450 °C. The deposited thin films were characterized by X‐ray diffraction (XRD) patterns, Raman spectra, scanning electron microscopy, energy dispersive X‐ray analysis (EDX) and atomic force microscopy. XRD studies of Cu‐doped FeS thin films at all the temperatures revealed formation of single‐phase FeS structure. With increasing substrate temperature from 250 to 450 °C, there was change in morphology from wafer‐like to cylindrical plate‐like. EDX analysis showed that the doping percentage of copper increased as the substrate temperature increased from 250 to 450 °C. Raman data supports the doping of copper in FeS films. Copyright © 2010 John Wiley & Sons, Ltd.     

Growth and characterization of ultrathin carbon films on electrodeposited Cu and Ni

Ultrathin carbon films were grown on different types of metallic substrates. Free‐standing foils of Cu and Ni were prepared by electroforming, and a pure Ni film was obtained by galvanic displacement on a Si wafer. Commercial foil of Ni 99.95% was used as a reference substrate. Carbon films were grown on these substrates by chemical vapour deposition in a CH₄‐H₂ atmosphere. Obtained films were characterized by Raman spectroscopy, X‐ray photoelectron spectroscopy (XPS), Auger electron spectroscopy, and ultraviolet photoemission spectroscopy. The XPS at grazing collection angle was used to determine the thickness of carbon films. Depending on the deposition parameters, the films of graphene or graphite were obtained on the different substrates. The uniformity of graphene and its distribution over the sample area were investigated from Raman data, optical images, and XPS chemical maps. The presence of graphene or graphite in the films was determined from the Raman spectra and Auger peak of C KVV. For this purpose, the D parameter, which is a fingerprint of carbon allotropes, was determined from C KVV spectra acquired by using X‐rays and electron beam. A formation of an intermediate layer of metal hydroxide was revealed in the samples with graphene overlayer.     

50 keV H+ ion beam irradiation of Al doped ZnO thin films: Studies of radiation stability for device applications

Thin films of Al doped ZnO (Al:ZnO) were deposited on two substrates (Si and glass) at room temperature and 300°C using DC magnetron sputtering. These films were bombarded with 50 keV H⁺ beam at several fluences. The pristine and ion beam irradiated films were analysed by X‐ray diffraction, Raman spectroscopy, scanning electron microscopy, and UV‐Vis spectroscopy. The X‐ray diffraction analysis, Hall measurements, Raman and UV‐Vis spectroscopy confirm that the structural and transport properties of Al:ZnO films do not change substantially with beam irradiation at chosen fluences. However, in comparison to film deposited at room temperature, the Al:ZnO thin film deposited at 300°C shows increased transmittance (from 70% to approximately 90%) with ion beam irradiation at highest fluence. The studies of surface morphology by scanning electron microscopy reveal that the ion irradiation yields smoothening of the films, which also increases with ion fluences. The films deposited at elevated temperature are smoother than those deposited at room temperature. In the paper, we discuss the interaction of 50 keV H⁺ ions with Al:ZnO films in terms of radiation stability in devices.     

Organic–inorganic nanocomposites of (2‐hydroxypropyl)cellulose as a precursor of nanocrystalline zinc oxide layers

The sol–gel method of synthesis of the hybrid nanocomposite films of ZnO/(2‐hydroxypropyl) cellulose (HPC) on silica glass is presented. The sol phases were prepared for different weight ratios of zinc acetate dihydrate to HPC in the presence of triethylamine (TEA). Raman spectrum of the mixture of ZnAc and HPC indicates coordinating interaction between zinc ion and HPC. The generation of ZnO nanoparticles in the HPC matrix proceeds in situ through the annealing of the gel phase at a temperature of 160°C. Identification of ZnO nanoparticles in the HPC matrix is done by using photoluminescence (PL), UV–Vis, and Raman spectroscopy. The films of ZnO/HPC nanocomposite are transparent in the visible light and show a higher energy value of absorption edge compared with ZnO in the bulk. Nanocrystalline films of ZnO were obtained by the calcination of ZnO/HPC nanocomposite at 500°C. ZnO films possess a good transparency for the visible light and high absorbance for UV light. Nanocrystallite sizes of ZnO particles were estimated from the X‐ ray lines broadening. The properties of ZnO layers were studied by the evaluation of PL, X‐ray investigation and atom force microscope (AFM) scanning, and the optical absorption edge. Copyright © 2008 John Wiley & Sons, Ltd.     

Synthesis,Characterization, Thermal Property of Si(c‐C5H9NH)4 and Its Potential as CVD Precursor for SiC Film

Silicon(IV) amide Si(c‐C₅H₉NH)₄ ( 1 ), was synthesized and characterized by ¹H, ¹³C, and ²⁹Si NMR spectroscopy, EI‐MS, elemental analysis, and X‐ray diffraction. Its thermal stability and volatility were also investigated. The as‐grown film, which was characterized by SEM, AFM, XRD and XPS, was deposited using 1 as single precursor through a low‐pressure chemical vapor deposition (LPCVD) process at a temperature as low as 600 °C. The results demonstrated that silicon(IV) amides can be promising single‐precursor for deposition of low‐temperature SiC films.     

Thin films of vanadium oxide grown on vanadium metal: oxidation conditions to produce V2O5 films for Li‐intercalation applications and characterisation by XPS,AFM, RBS/NRA

Thin films of vanadium oxide were grown on vanadium metal surfaces (i) in air at ambient conditions, (ii) in 5 mM H₂SO₄ (aq), pH 3, (iii) by thermal oxidation at low oxygen pressure (10^?5 mbar) at temperatures between 350 and 550 °C and (iv) at near‐atmospheric oxygen pressure (750 mbar) at 500 °C. The oxide films were investigated by atomic force microscopy (AFM), X‐ray photoelectron spectroscopy (XPS), X‐Ray diffraction (XRD) and Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). The lithium intercalation properties were studied by cyclic voltammetry (CV). The results show that the oxide films formed in air at room temperature (RT), in acidic aqueous solution, and at low oxygen pressure at elevated temperatures are composed of V₂O₃. In air and in aqueous solution at RT, the oxide films are ultra‐thin and hydroxylated. At 500 °C, nearly atmospheric oxygen pressure is required to form crystalline V₂O₅ films. The oxide films grown at pO₂ = 750 mbar for 5 min are about 260‐nm thick, and consist of a 115‐nm outer layer of crystalline V₂O₅. The inner oxide is mainly composed of VO₂. For all high temperature oxidations, the oxygen diffusion from the oxide film into the metal matrix was considerable. The oxygen saturation of the metal at 450 °C was found, by XPS, to be 27 at.% at the oxide/metal interface. The well‐crystallized V₂O₅ film, formed by oxidation for 5 min at 500 °C and 750 mbar O₂, was shown to have good lithium intercalation properties and is a promising candidate as electrode material in lithium batteries. Copyright © 2005 John Wiley & Sons, Ltd.     

Nanostructured ZrO2 and Zr‐C‐N Coatings from Chemical Vapor Deposition of Metal‐Organic Precursors

Nanocrystalline zirconium carbonitride (Zr‐C‐N) and zirconium oxide (ZrO₂) films were deposited by chemical vapor deposition (CVD) of zirconium‐tetrakis‐diethylamide (Zr(NEt₂)₄) and ‐tert‐butyloxide (Zr(OBu^t)₄), respectively. The films were deposited on iron substrates and characterized by scanning electron microscopy (SEM), X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). The Zr‐C‐N films show blue, golden brown or bronze colours, with colour stability depending upon the precursor composition (pure metal amide or mixed with Et₂NH). The deposition temperature showed no pronounced effect on the granular morphology of the Zr‐C‐N films. The XRD data of the films correspond to the formation of carbonitride phase whereas the XPS analyses revealed a strong surface oxidation and incorporation of oxygen in the film. The films deposited using a mixture of Zr(NEt₂)₄ and Et₂NH showed higher N content, better adhesion and scratch resistance when compared to films obtained from the CVD of pure Zr(NEt₂)₄. Subject to the precursor composition and deposition temperature (550‐750 °C), the microhardness values of Zr‐C‐N films were found to be in the range 2.11‐5.65 GPa. For ZrO₂ films, morphology and phase composition strongly depend on the deposition temperature. The CVD deposits obtained at 350 °C show tetragonal ZrO₂ to be the only crystalline phase. Upon increasing the deposition temperature to 450 °C, a mixture of tetragonal and monoclinic modifications was formed with morphology made up of interwoven elongated grains. At higher temperatures (550 and 650 °C), pure monoclinic phase was obtained with facetted grains and developed texture.     

Nitridation of V5Al8 films with NH3 by Rapid Thermal Processing (RTP)

V₅Al₈ films (thickness about 100 nm) were deposited on sapphire substrates by RF‐sputtering and nitridated with NH₃ at 600‐1250 °C (1 min) in a RTP system. The as deposited and nitridated films were investigated by ESCA (electron spectroscopy for chemical analysis), XRD (X‐ray diffraction), XRR (X‐ray reflectometry), AFM (atomic force microscopy) and SEM (scanning electron microscopy). Formation of an aluminum nitride layer at the surface and precipitation of V(Al) in the bulk was found. In the temperature regime from 600 °C to 900 °C a considerable amount of oxygen is incorporated in the aluminum nitride layer. The roughness of the surface increased with increasing temperature and at 1250 °C a partially detaching of the AlN layer could be observed.     

Structure and Dielectric Properties of NiTiO3 Powders Synthesized by the Modified Sol–Gel Method

This study reports the synthesis of nickel titanate (NiTiO₃) powders by using the modified sol‐gel method, with nickel acetate tetrahydrate as the nickel source, titanium isopropoxide as the titanium source, and 2‐methoxyethanol as the solvent, followed by post‐heat treatment in air at temperatures ranging from 500 °C to 900 °C. The characteristics of powders were determined by X‐ray diffraction (XRD), FT‐infrared spectroscopy (FT‐IR), ultraviolet/visible spectroscopy (UV/Vis), and Raman spectroscopy. The particle size and surface area of the powders were also measured. The results indicated that single‐phase NiTiO₃ can be prepared using the modified sol‐gel method, followed by post‐heat treatment at the relatively low temperature of 550 °C. The crystallite sizes and particle sizes of NiTiO₃ powders increase in conjunction with the post‐heat treatment temperatures. However, the surface area of the powders shrinks as the post‐heat treatment temperatures increase. The dielectric constants of NiTiO₃ powders, based on the capacitance‐voltage analysis, are within a range of 13.2 to 17.8.     

Well Oriented ZnO Nanorods Array: Negative Resistance and Optical Switching

Well‐oriented ZnO nanorods (NRs) arrays were grown on Si, alumina, quartz, and FTO substrates through a ZnO seed layer followed by low temperature wet chemical process. The influence of sputtered ZnO seed layer thickness (100, 50, 32, and 16 nm), annealing temperature and CuO_x coverage on the characteristics of ZnO NRs were investigated in this study. The crystalline structural, chemical, morphological, optical, and electrical properties of ZnO NRs arrays were studied by X‐ray diffraction (XRD), field emission‐ scanning electron microscopy equipped by energy dispersive X‐ray spectroscopy (FE‐SEM/EDX), Raman scattering, UV/Vis ‐ near IR absorption spectroscopy and current‐voltage characteristic. XRD and Raman spectra measurement revealed that the synthesize ZnO displayed hexagonal wurtzite structure. The individual rod diameter, density, and orientation can be controlled by varying the seed layer thickness. The mean diameter and maximum length of ZnO NRs are around 55–66 nm and 282 nm, respectively. ZnO NRs/ ZnO thin film structure shows optical switching and negative differential resistance behavior as applicable to ON/OFF gate and memory devices.     

Structural and electrical properties of Li doped ZnO under Ar/H2 atmosphere

Thin films of ZnO were grown by the sol–gel method using spin-coating technique on (0001) sapphire substrates. The effect of doping under Ar/H₂ atmosphere on the structural and electrical properties of ZnO was investigated by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), I–V characterization, Hall effect and micro-photoluminescence. The films that were annealed at 600 °C in Ar/H₂ (95/5) % atmosphere showed (002) a predominant orientation. The crystalline nature of 2 mol.  % of Li doped films were better when compared to 1 mol.  % of Li doped films. The incorporation of Li in ZnO lattice was confirmed by X-ray photoelectron spectroscopy, and micro-photoluminescence. Hall effect measurements and I–V characterization of the Li doped ZnO thin films exhibited a better p-type behavior.     

Investigation of Fe−Ni Mixed‐Oxide Catalysts for the Reduction of NO by CO: Physicochemical Properties and Catalytic Performance

A series of Fe?Ni mixed‐oxide catalysts were synthesized by using the sol–gel method for the reduction of NO by CO. These Fe?Ni mixed‐oxide catalysts exhibited tremendously enhanced catalytic performance compared to monometallic catalysts that were prepared by using the same method. The effects of Fe/Ni molar ratio and calcination temperature on the catalytic activity were examined and the physicochemical properties of the catalysts were characterized by using XRD, Raman spectroscopy, N₂‐adsorption/‐desorption isotherms, temperature‐programmed reduction with hydrogen (H₂‐TPR), temperature‐programmed desorption of nitric oxide (NO‐TPD), and X‐ray photoelectron spectroscopy (XPS). The results indicated that the reduction behavior, surface oxygen species, and surface chemical valence states of iron and nickel in the catalysts were the key factors in the NO elimination. Fe_0.5Ni_0.5O_x that was calcined at 250 °C exhibited excellent catalytic activity of 100 % NO conversion at 130 °C and a lifetime of more than 40 hours. A plausible mechanism for the reduction of NO by CO over the Fe?Ni mixed‐oxide catalysts is proposed, based on XPS and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) analyses.     

Characterization of siloxane films on titanium substrate derived from three aminosilanes

The aim of this investigation was to study the siloxane, ? Si? O? Si? , film formation on Ti substrate by using mono‐, bis‐ and tris‐aminosilanes. The ultimate goal was to obtain a smooth, well‐organized and stable siloxane film with suitable surface energy. Such films are expected to perform well in adhering resins to dental metal alloys when the films contain reactive functional groups. Aminosilanes were prepared as 0.5 vol.% solutions in dilute ethanol (50 vol.% ethanol in deionized water), with their natural pH of ～ 9. The substrates were silanized in two ways: silane was allowed to react at room temperature or was cured for 1 h at 110°C. The surface characterization was carried out by reflectance–absorbance Fourier transform infrared spectroscopy (RA‐FTIR), x‐ray photoelectron spectroscopy (XPS), contact angle measurement and atomic force microscopy (AFM). Siloxane film thickness measurements were not made. According to spectral analysis, all silanes indicated covalent bond formation with titanium. ?Si? O? Ti? and ?Si? O? Si? bonds were clearly seen in the spectra, suggesting that chemical retention had taken place. After curing at elevated temperature, the spectral bands seemed to be stronger than those on samples cured at room temperature. Curing of hydrolyzed silanes at elevated temperature seemed to enhance the siloxane layer formation, derived from aminosilanes, on the Ti substrate. This might have an influence on the hydrolytic stability of organosilane‐promoted adhesion between Ti and dental resins. Copyright © 2004 John Wiley & Sons, Ltd.     

Thickness and temperature‐dependent study of Co/Si interface

Thin films of cobalt (10, 40, and 100 nm) are deposited on Si substrate by electron beam physical vapor deposition technique. After deposition, 4 pieces from each of the wafers of silicon substrate were cut and annealed at a temperature of 200°C, 300°C, and 400°C for 2 hours each, separately. X‐ray diffraction, atomic force microscopy, and transmission electron microscopy (TEM) are used to study the structural and morphological characteristics of the deposited films. To obtain TEM images, Co films are deposited on Cu grids; so far, no such types of TEM images of Co films are reported. Structural studies confirm nanocrystalline nature with hexagonal close packed structure of the deposited Co film at lower thickness, while at higher thickness, film structure transforms to amorphous with lower surface roughness value. The particle sizes in all the cases are in the range of 3 to 5 nm. Micro‐Raman spectroscopy is also used to study the phase formation and chemical composition as a function of thickness and temperature. The results confirm that the grown films are of good quality and free from any impurity. Studies show the silicide formation at the interface during deposition. The appearance of new band at 1550 cm⁻¹ as a result of annealing indicates the structural transformation from CoSi to CoSi₂, which further enhances at higher annealing temperatures.     

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%.     

Influence of thermal annealing on the structural and optical properties of maghemite (γ‐Fe2O3) nanoparticle thin films

In this study, maghemite (γ‐Fe₂O₃) nanoparticles were initially synthesized via chemical co‐precipitation and then deposited by spray pyrolysis as thin films on white glass substrates. The thin films were annealed for 8 h at 400, 450, 500, 550, and 600 °C in an oven. The structural studies of maghemite nanoparticles were carried out using X‐ray diffractometer. Structural properties that we investigated by X‐ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, SEM, and Energy dispersive X‐ray analysis (EDS). Optical properties of the samples were also investigated by ultraviolet‐visible (UV–vis) spectroscopy. The results showed that maghemite nanoparticles have crystalline structure with domain that increases in size with increasing annealing temperature. The optical band gap values were found to reduce from 2.9 to 2.4 eV with increase in annealing temperature. Copyright © 2015 John Wiley & Sons, Ltd.     

Template‐free Fabrication of Hierarchical Macro‐/mesoporous N‐doped TiO2/graphene Oxide Composites with Enhanced Visible‐light Photocatalytic Activity

Hierarchical macro‐/mesoporous N‐doped TiO₂/graphene oxide (N‐TiO₂/GO) composites were prepared without using templates by the simple dropwise addition mixed solution of tetrabutyl titanate and ethanol containg graphene oxide (GO) to the ammonia solution, and then calcined at 350 °C. The as‐prepared samples were characterized by scanning electron microscopy (SEM), Brunauer‐Emmett‐Teller (BET) surface area, X‐ray diffraction (XRD), Raman spectroscopy, X‐ray photoelectron spectroscopy (XPS), and UV‐Vis absorption spectroscopy. The photocatalytic activity was evaluated by the photocatalytic degradation of methyl orange in an aqueous solution under visible‐light irradiation. The results show that N‐TiO₂/GO composites exhibited enhanced photocatalytic activity. GO content exhibited an obvious influence on photocatalytic performance, and the optimal GO addition content was 1 wt%. The enhanced photocatalytic activity could be attributed to the synergetic effects of three factors including the improved visible light absorption, the hierarchical macro‐mesoporous structure, and the efficient charge separation by GO.     

A facile approach to hexagonal ZnO nanorod assembly

Nanocrystalline ZnO nanorods were successfully grown by ultrasonication using an acidic ethanolic zinc acetate precursor solution followed by a flow coating process and annealing at 600 °C. The ZnO nanorods obtained were hexagonal in shape and showed a high degree of uniformity in size and distribution. These samples were characterized by X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and Raman spectrophotometry and the results are discussed. This approach appears to be the easiest way to fabricate bulk ZnO nanorods.     

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.