The influence of substrate temperature variation on tungsten oxide thin film growth in an HFCVD system

Tungsten oxide (WO₃) thin films were deposited by a modified hot filament chemical vapor deposition (HFCVD) technique using Si (1 0 0) substrates. The substrate temperature was varied from room temperature to 430 °C at an interval of 100 °C. The influence of the substrate temperature on the structural and optical properties of the WO₃ films was studied. X-ray diffraction and Raman spectra show that as substrate temperature increases the film tends to crystallize from the amorphous state and the surface roughness decreases sharply after 230 °C as confirmed from AFM image analysis. Also from the X-ray analysis it is evident that the substrate orientation plays a key role in growth. There is a sharp peak for samples on Si substrate due to texturing. The film thickness also decreases as substrate temperature increases. UV-vis spectra show that as substrate temperature increases the film property changes from metallic to insulating behavior due to changing stoichiometry, which was confirmed by XPS analysis.     

Surface chemical states of barium zirconate titanate thin films prepared by chemical solution deposition

Ba(Zr_0.05Ti_0.95)O₃ (BZT) thin films grown on Pt/Ti/SiO₂/Si(1 0 0) substrates were prepared by chemical solution deposition. The structural and surface morphology of BZT thin films has been studied by X-ray diffraction (XRD) and scanning electron microscope (SEM). The results showed that the random oriented BZT thin film grown on Pt/Ti/SiO₂/Si(1 0 0) substrate with a perovskite phase. The SEM surface image showed that the BZT thin film was crack-free. And the average grain size and thickness of the BZT film are 35 and 400 nm, respectively. Furthermore, the chemical states and chemical composition of the films were determined by X-ray photoelectron spectroscopy (XPS) near the surface. The XPS results show that Ba, Ti, and Zr exist mainly in the forms of BZT perovskite structure.     

The study of novel Fe3O4@γ-Fe2O3 core/shell nanomaterials with improved properties

The surface structure of the iron oxide nanoparticles obtained by the co-precipitation method has been investigated, and a thin layer of α-FeOOH absorbed on surface of the nanoparticle is confirmed by analyses of Fourier transform infrared (FTIR), X-ray photoelectron spectra (XPS) and surface photovoltage spectroscopy (SPS). After annealed at 400 °C, the α-FeOOH can be converted to γ-Fe₂O₃. The simple-annealed procedure resulted in the formation of Fe₃O₄@γ-Fe₂O₃ core/shell structure with improved stability and a higher magnetic saturation value, and also the simple method can be used to obtain core/shell structure in other similar system.     

Pd adsorption on Si(1 1 3) surface: STM and XPS study

Pd-induced surface structures on Si(1 1 3) have been studied by scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS). In the initial process of the Pd adsorption below 0.10 ML, Pd silicide (Pd₂Si) clusters are observed to form randomly on the surface. By increasing the Pd coverage to 0.10 ML, the clusters cover the entire surface, and an amorphous layer is formed. After annealing the Si(1 1 3)-Pd surface at 600 °C, various types of islands and chain protrusions appears. The agglomeration, coalescence and crystallization of these islands are observed by using high temperature (HT-) STM. It is also found by XPS that the islands correspond to Pd₂Si structure. On the basis of these results, evolution of Pd-induced structures at high temperatures is in detail discussed.     

Synthesis and electrochemical characteristics of Ta-N thin films fabricated by cathodic arc deposition

Ta-N thin films were deposited on AISI 317L stainless steel (SS) substrates by cathodic arc deposition (CAD) at substrate biases of −50 and −200 V. The as-deposited films were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray analysis (EDX). The results show that stoichiometric TaN with hexagonal lattice (3 0 0) preferred orientation was achieved at the bias of −200 V. On the other hand, Ta-rich Ta-N thin film deposited at −50 V shows amorphous nature. According to the XPS result, Ta element in the films surface exist in bonded state, including the Ta-N bonds characterized by the doublet (Ta 4f_7/2 = 23.7 eV and Ta 4f_5/2 = 25.7 eV). Electrochemical properties of the Ta-N coated stainless steel systems were investigated using potentiodynamic polarization and electrochemical impedance spectroscope (EIS) in Hank's solution at 37 °C. For the Ta-N coated samples, the corrosion current (i_corr) is two or three orders of magnitude lower than that of the uncoated ones, indicating a significantly improved corrosion resistance. Growth defects in the Ta-N thin films produced by CAD, however, play a key role in the corrosion process, especially the localised corrosion. Using the polarization fitting and the EIS modelling, we compared the polarization resistance (R_p) and the porosity (P) of the Ta-N coatings deposited at different biases. It seems that Ta-N film with comparatively lower bias (−50 V) shows better corrosion behavior in artifical physiological solution. That may be attributed to the effect of ion bombarding, which can be modulated by the substrate bias.     

Effect of calcination temperature on the morphology and surface properties of TiO2 nanotube arrays

Well-ordered TiO₂ nanotube arrays were prepared by electrochemical anodization of titanium in aqueous electrolyte solution of H₃PO₄ + NH₄F at a constant voltage of 20 V for 3 h, followed by calcined at various temperatures. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS) and Photoluminescence (PL) were used to characterize the samples. The results showed that the as-prepared nanotube arrays before being calcined were amorphous and could transform to anatase phase at a heat treatment temperature higher than 400 °C. As the calcination temperatures increased, crystallization of anatase phase enhanced and rutile phase appeared at 600 °C. However, further increasing the calcination temperature would cause the collapse of nanotube arrays. PL intensity of the nanotube arrays annealed at 500 °C was the lowest, which was probably ascribed to better crystallization together with fewer surface defects of the nanotube arrays.     

Preparation of activated carbon from cherry stones by chemical activation with ZnCl2

Cherry stones (CS), an industrial product generated abundantly in the Valle del Jerte (Cáceres province, Spain), were used as precursor in the preparation of activated carbon by chemical activation with ZnCl₂. The influence of process variables such as the carbonisation temperature and the ZnCl₂:CS ratio (impregnation ratio) on textural and chemical-surface properties of the products obtained was studied. Such products were characterised texturally by adsorption of N₂ at −196 °C, mercury porosimetry and density measurements. Information on the surface functional groups and structures of the carbons was provided by FT-IR spectroscopy. Activated carbon with a high development of surface area and porosity is prepared. When using the 4:1 impregnation ratio, the specific surface area (BET) of the resultant carbon is as high as 1971 m² g⁻¹. The effect of the increase in the impregnation ratio on the porous structure of activated carbon is stronger than that of the rise in the carbonisation temperature, whereas the opposite applies to the effect on the surface functional groups and structures.     

Effect of surface fluorination on the photocatalytic and photo-induced hydrophilic properties of porous TiO2 films

Porous surface-fluorinated TiO₂ (F-TiO₂) films were prepared through PEG modified sol-gel method and surface fluorination. The as-prepared films were characterized with XRD, FTIR, AFM, XPS and UV-vis DRS. The effects of surface fluorination on the photocatalytic activity and hydrophilicity of porous TiO₂ film were studied by photocatalytic degradation of rhodamine B (RhB) as well as water contact angle (CA) on porous TiO₂ film. The results showed that the surface fluorination increased the adsorption of RhB on the porous TiO₂ film and enhanced the photocatalytic degradation of RhB. The concentration and pH of NaF solutions affected much the photocatalytic activity of porous TiO₂ film. Porous F-TiO₂ film prepared in 40 mM NaF solution at pH 4.0 showed the highest photocatalytic activity. Because of its porous structure, the porous F-TiO₂ film had original water CA of 22.7°, which is much smaller than that of normal F-TiO₂ film. Under UV light irradiation, the water CA of porous F-TiO₂ film decreased to 5.1° in 90 min.     

AlCl3-induced crystallization of amorphous silicon thin films

It is reported that the direct contact between Al and amorphous silicon (a-Si) enhances the crystallization of a-Si films. But the polycrystalline silicon (poly-Si) films crystallized by the direct contact of Al metal film suffer the problems of rough surface. In our study, we utilized the AlCl₃ vapor during the a-Si films deposition instead of Al metal film to enhance crystallization. X-ray diffraction (XRD) shows that the AlCl₃ vapor so successfully enhanced the crystallization of a-Si films that the crystallization was completed in 5 h at 540 °C. And the orientation of the poly-Si film deposited with AlCl₃ vapor is much more random than that of annealed with Al metal under layer. But the average grain size is much larger than that. Moreover, the surface of the AlCl₃-induced crystallized poly-Si film was much smoother than that of the Al-induced poly-Si film. The Al and Cl incorporation into the poly-Si film was confirmed using X-ray photoelectron spectroscopy (XPS) and found that the quantity of Al and Cl incorporated into the Si film was below the detection limit of XPS.     

Surface modification of cobalt-chromium-tungsten-nickel alloy using octadecyltrichlorosilanes

Cobalt-chromium (Co-Cr) alloys have been extensively used for medical implants because of their excellent mechanical properties, corrosion resistance, and biocompatibility. This first time study reports the formation and stability of self-assembled monolayers (SAMs) on a Co-Cr-W-Ni alloy. SAMs of octadecyltrichlorosilanes (OTS) were coated on sputtered Co-Cr-W-Ni alloy thin film and bulk Co-Cr-W-Ni alloy. OTS SAM coated alloy specimens were characterized using contact angle goniometry, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM). Contact angle analysis and FTIR suggested that ordered monolayers were coated on both sputtered and bulk alloy. XPS suggested the selective dissolution of cobalt from the alloy during the formation of OTS SAM. The bonding between the alloy and the OTS SAM was mainly attributed to Si-O-Cr and Si-O-W covalent bonds and a smaller contribution from Si-O-Co bonds. AFM images showed the distribution of islands of monolayers coated on the alloy. The height of monolayers in majority of the islands was closer to the theoretical length of fully extended OTS molecules oriented perpendicular to the surface. The stability of OTS SAM was investigated in tris-buffered saline at 37 °C for up to 7 days. Contact angle, FTIR, and XPS collectively confirmed that the monolayers remain ordered and bound to the alloy surface under this condition. This study shows that Co-Cr alloys can be surface modified using SAMs for potential biomedical applications.     

Structural and morphological characterization of TiO2 nanostructured films grown by nanosecond pulsed laser deposition

TiO₂ has attracted a lot of attention due to its photocatalytic properties and its potential applications in environmental purification and self cleaning coatings, as well as for its high optical transmittance in the visible-IR spectral range, high chemical stability and mechanical resistance. In this paper, we report on the growth of TiO₂ nanocrystalline films on Si (1 0 0) substrates by pulsed laser deposition (PLD). Rutile sintered targets were irradiated by KrF excimer laser (λ = 248 nm, pulse duration ∼30 ns) in a controlled oxygen environment and at constant substrate temperature of 650 °C. The structural and morphological properties of the films have been studied for different deposition parameters, such as oxygen partial pressure (0.05-5 Pa) and laser fluence (2- 4 J/cm²). X-ray diffraction (XRD) shows the formation of both rutile and anatase phases; however, it is observed that the anatase phase is suppressed at the highest laser fluences. X-ray photoelectron spectroscopy (XPS) measurements were performed to determine the stoichiometry of the grown films. The surface morphology of the deposits, studied by scanning electron (SEM) and atomic force (AFM) microscopies, has revealed nanostructured films. The dimensions and density of the nanoparticles observed at the surface depend on the partial pressure of oxygen during growth. The smallest particles of about 40 nm diameter were obtained for the highest pressures of inlet gas.     

Laser-induced forward transfer technique for maskless patterning of amorphous V2O5 thin film

A laser-induced forward transfer technique has been applied for the maskless patterning of amorphous V₂O₅ thin films. A sheet beam of a frequency doubled (SHG) Q-switched Nd:YAG laser was irradiated on a transparent glass substrate (donor), the rear surface of which was pre-coated with a vacuum-deposited V₂O₅ 180 nm thick film was either in direct contact with a second glass substrate (receiver) or a 0.14 mm air-gap was maintained between the donor film and the receiving substrate. Clear, regular stripe pattern of the laser-induced transferred film was obtained on the receiver. The pattern was characterized using X-ray diffraction (XRD), optical absorption spectroscopy, scanning electron microscopy (SEM), energy dispersive analysis of X-ray (EDAX), atomic force microscopy (AFM), etc.     

Weathering properties of treated southern yellow pine wood examined by X-ray photoelectron spectroscopy, scanning electron microscopy and physical characterization

In this study the weathering behavior of southern yellow pine (SYP) wood samples pretreated in different solutions has been examined using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and various types of physical characterization regarding material loss and discoloration. The treatment solutions include water as a control, a commercially available water repellent (WR) wood treating additive and polyethylene glycol (PEG) products including PEG PLUS™, PEG 8000 solutions and Compound 20M in varying concentrations. All contained the wood preservative chromated copper arsenate (CCA). One sample was treated with a CCA solution only. The treatments were carried out at 20 °C and 150 psig for 1/2 h after exposure to vacuum (28 mmHg) for 15 min. Simulated weathering was achieved in an Atlas 65-W Weather-Ometer for 2000 h with both light and dark periods and rain. The temperature ranged from 23 °C during the dark cycle to 35 °C during the light cycle. With weathering the XPS O/C ratios increase due to oxidation of the surface. Exposure to UV light results in bond breakage and reaction with oxygen in the presence of air to form organic functional groups such as , , CO and/or O-C-O. These oxidized products can protect the underlying wood from deterioration if they are insoluble in water and remain on the surface as a protective coating. If soluble, rain washes the compounds away and assists in the degradation. Correlated changes are observed in the XPS O/C ratios, the high-resolution XPS C 1s spectra, the SEM micrographs and physical measurements including thickness alteration, weight loss, and discoloration by yellowing or whitening of the weathered wood. The PEG treatments are effective in protecting wood with the 2% PEG PLUS treatment providing the best weathering behavior similar to that of the CCA treatment. The WR and water treatments yield the poorest weathering properties.     

Fabrication, morphology, and photoluminescence properties of GaN nanowires and nanorods by ammoniating Ga2O3/V films on Si(1 1 1)

GaN nanowires and nanorods have been successfully synthesized on Si(1 1 1) substrates by magnetron sputtering through ammoniating Ga₂O₃/V films at 900 °C in a quartz tube. X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectrum were carried out to characterize the structure, morphology, and photoluminescence properties of GaN sample. The results show that the GaN nanowires and nanorods with pure hexagonal wurtzite structure have good emission properties. The growth direction of nanostructures is perpendicular to the fringes of (1 0 1) plane. The growth mechanism is also briefly discussed.     

Preparation of activated carbons from cherry stones by activation with potassium hydroxide

Using cherry stones, the preparation of activated carbon has been undertaken in the present study by chemical activation with potassium hydroxide. A series of KOH-activated products was prepared by varying the carbonisation temperature in the 400-900 °C range. Such products were characterised texturally by gas adsorption (N₂, −196 °C), mercury porosimetry, and helium and mercury density measurements. FT-IR spectroscopy was also applied. The carbons prepared as a rule are microporous and macroporous solids. The degree of development of surface area and porosity increases with increasing carbonisation temperature. For the carbon heated at 900 °C the specific surface area (BET) is 1624 m² g⁻¹, the micropore volume is 0.67 cm³ g⁻¹, the mesopore volume is 0.28 cm³ g⁻¹, and the macropore volume is 1.84 cm³ g⁻¹.     

Functionalization of lamellar molybdenum disulphide nanocomposite with gold nanoparticles

This work explores the functionalization of an organic-inorganic MoS₂ lamellar compound, prepared by a chemical liquid deposition method (CLD), that has an interlamellar distance of ∼5.2 nm, using clusters of gold nanoparticles. The gold nanoparticles have a mean diameter of 1.2 nm, a stability of ∼85 days, and a zeta potential measured to be ζ = −6.8 mV (solid). The nanoparticles are localized in the hydrophilic zones, defined by the presence of amine groups of the surfactant between the lamella of MoS₂. SEM, TEM, EDAX and electron diffraction provide conclusive evidence of the interlamellar insertion of the gold nanoparticles in the MoS₂.     

Preparation and textural characterisation of activated carbon from vine shoots (Vitis vinifera) by H3PO4—Chemical activation

An abundant and low-cost agricultural waste as vine shoots (Vitis vinifera) (VS), which is generated by the annual pruning of vineyards, has been used as raw material in the preparation of powder activated carbon (AC) by the method of chemical activation with phosphoric acid. After size reduction, VS were impregnated for 2 h with 60 wt.% H₃PO₄ solution at room temperature, 50 and 85 °C. The three impregnated products were carbonised at 400 °C. The product impregnated at 50 °C was heated either first at 150-250 °C and then at 400 °C or simply at 350-550 °C in N₂ atmosphere. The time of isothermal treatment after each dynamic heating was 2 h. The carbons were texturally characterised by gas adsorption (N₂, −196 °C), mercury porosimetry, and density measurements. FT-IR spectroscopy was also applied. Better developments of surface area and microporosity are obtained when the impregnation of VS with the H₃PO₄ solution is effected at 50 °C and for the products heated isothermally at 200 and 450 °C. The mesopore volume is also usually higher for the products impregnated and heated at intermediate temperatures.     

Ordered mesoporous silica materials (SBA-15) with good heat-resistant magnetism

A series of highly ordered mesoporous materials (CF-SBA-15) with heat-resistant magnetism have been successfully prepared from impregnation of cobalt salt, iron salt, and citric acid with as-synthesized SBA-15. XRD and N₂ isotherms indicate that these materials have highly ordered hexagonal mesoporous symmetry and open pore systems. The measurement of magnetic property shows that these materials are ferromagnetic even if calcined at 550 °C for 10 h in air, indicating their good heat-resistant magnetism. These results would be very important for recycle and regeneration of adsorbents and catalysts in practical applications. Moreover, this method may be useful for other mesoporous materials with thermally stable magnetism from a combination of other mesoporous materials such as MCM-41 with magnetic nanoparticles of MnFe₂O₄ and NiFe₂O₄.     

Short-time plasma surface modification of HDPE powder in a Plasma Downer Reactor - process, wettability improvement and ageing effects

The effectiveness of improving the wettability of HDPE powders within less than 0.1 s by plasma surface modification in a Plasma Downer Reactor is investigated. A correlation is revealed between the XPS results (O/C-ratio) and the wettability (contact angle, polar surface tension by capillary rise method). The O₂-content in the plasma feed gas has been adjusted for best wettability properties. XPS results indicate the formation of CO and COOH functional groups on the powder surface. The O/C-ratio increased from 0.0 (no oxygen on the non-treated powder) up to 0.15 for the plasma treated HDPE powder surface. With pure O₂-plasma treatment, a water contact angle reduction from >90° (no water penetration into the untreated PE powder) down to 65° was achieved. The total surface free energy increased from 31.2 to 45 mN/m. Ageing of treated powders occurs and proceeds mostly within the first 7 days of storage. Contact angle measurements and O1s/O2s intensity ratio data support that ageing is mainly a diffusion-controlled process. Nevertheless, XPS results show the presence of oxygen functional groups even after 40 days, which explains why the powder is still dispersible in water without any addition of surfactants.     

Effects of the sputtering time of ZnO buffer layer on the quality of GaN thin films

ZnO thin films with different thickness (the sputtering time of ZnO buffer layers was 10 min, 15 min, 20 min, and 25 min, respectively) were first prepared on Si substrates using radio frequency magnetron sputtering system and then the samples were annealed at 900 °C in oxygen ambient. Subsequently, a GaN epilayer about 500 nm thick was deposited on ZnO buffer layer. The GaN/ZnO films were annealed in NH₃ ambient at 950 °C. X-ray diffraction (XRD), atom force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL) were used to analyze the structure, morphology, composition and optical properties of GaN films. The results show that their properties are investigated particularly as a function of the sputtering time of ZnO layers. For the better growth of GaN films, the optimal sputtering time is 15 min.