Influence of heating rate on the crystalline properties of 0.7BiFeO3-0.3PbTiO3 thin films prepared by sol-gel process

0.7BiFeO₃-0.3PbTiO₃ (BFPT7030) thin films were deposited on SiO₂/Si substrates by sol-gel process. The influence of heating rate on the crystalline properties of BFPT7030 thin films were studied by X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). XRD patterns of the films showed that a pure perovskite phase exists in BFPT7030 films annealed by rapid thermal annealing (RTA) technique. SEM and AFM observations demonstrated that the BFPT7030 films annealed by RTA at 700 °C for 90 s with the heating rate of 1 °C s⁻¹ could show a dense, crack-free surface morphology, and the films’ grains grow better than those of the films annealed by RTA at the same temperature with other heating rates. XPS results of the films indicated that the ratio of Fe³⁺:Fe²⁺ is about 21:10 and 9:5 for the films annealed by RTA at 700 °C for 90 s with the heating rate of 1 and 20 °C s⁻¹, respectively. That means the higher the heating rate, the higher the concentration of Fe²⁺ in the BFPT7030 thin films.     

rf reactive co-sputtered Au-Ag alloy nanoparticles in SiO2 thin films

We have studied formation of Au-Ag alloy nanoparticles in sputtered SiO₂ thin films. Silica thin films containing Au-Ag nanoparticles were deposited on quartz substrates using rf reactive magnetron co-sputtering technique. The films heat-treated in reducing Ar + H₂ atmosphere at different temperatures. They were analyzed by using UV-vis spectrophotometry, atomic force microscopy and X-ray photoelectron spectroscopy (XPS) methods for their optical, surface morphological as well as structural and chemical properties. The optical absorption of the Au-Ag alloy nanoparticles illustrated one plasmon resonance absorption peak located at 450 nm between the absorption bands of pure Au and Ag nanoparticles at 400 and 520 nm, respectively, for the thin films annealed at 800 °C. XPS results showed that the alloys were in metallic state, and they had a greater tendency to lose electrons as compared to their corresponding monometallic state. Using lateral force microscopy analysis, we have found that the alloy particles were uniformly distributed on the surface with grain size of about 20 nm.     

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.     

Effect of annealing on electrical resistivity of rf-magnetron sputtered nanostructured SnO2 thin films

Tin oxide (SnO₂) thin films were deposited by radio frequency (RF) magnetron sputtering on clean corning glass substrates. These films were then annealed for 15 min at various temperatures in the range of 100-500°C. The films were investigated by studying their structural and electrical properties. X-ray diffraction (XRD) results suggested that the deposited SnO₂ films were formed by nanoparticles with average particle size in the range of 23-28 nm. XRD patterns of annealed films showed the formation of small amount of SnO phase in the matrix of SnO₂. The initial surface RMS roughness measured with atomic force microscopy (AFM) was 25.76 nm which reduces to 17.72 nm with annealing. Electrical resistivity was measured as a function of annealing temperature and found to lie between 1.25 and 1.38 mΩ cm. RMS roughness and resistivity show almost opposite trend with annealing.     

Electron beam evaporated LaF3 thin films prepared by different temperatures and deposition rates

LaF₃ thin films were prepared by electron beam evaporation with different temperatures and deposition rates. Microstructure properties including crystalline structure and surface roughness were investigated by X-ray diffraction (XRD) and optical profilograph. X-ray photoelectron spectroscopy (XPS) was employed to study the chemical composition of the films. Optical properties (transmittance and refractive index) and laser induce damage threshold (LIDT) at 355 nm of the films were also characterized. The effects of deposition rate and substrate temperature on microstructure, optical properties and LIDT of LaF₃ thin films were discussed, respectively.     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Microstructural and surface property variations due to the amorphous region formed by thermal annealing in Al-doped ZnO thin films grown on n-Si (1 0 0) substrates

X-ray diffraction (XRD) patterns revealed that the as-grown and annealed Al-doped ZnO (AZO) films grown on the n-Si (1 0 0) substrates were polycrystalline. Transmission electron microscopy (TEM) images showed that bright-contrast regions existed in the grain boundary, and high-resolution TEM (HRTEM) images showed that the bright-contrast regions with an amorphous phase were embedded in the ZnO grains. While the surface roughness of the AZO film annealed at 800 °C became smoother, those of the AZO films annealed at 900 and 1000 °C became rougher. XRD patterns, TEM images, selected-area electron diffraction patterns, HRTEM images, and atomic force microscopy (AFM) images showed that the crystallinity in the AZO thin films grown on the n-Si (1 0 0) substrates was enhanced resulting from the release in the strain energy for the AZO thin films due to thermal annealing at 800 °C. XRD patterns and AFM images show that the crystallinity of the AZO thin films annealed at 1000 °C deteriorated due to the formation of the amorphous phase in the ZnO thin films.     

Structural, optical and photoelectrochemical characterization of CdS nanowire synthesized by chemical bath deposition and wet chemical etching

Nanocrystalline thin films of CdS have been grown onto flexible plastic and titanium substrates by a simple and environmentally benign chemical bath deposition (CBD) method at room temperature. The films consist of clusters of CdS nanoparticles. The clusters of CdS nanoparticles in the films were successfully converted into nanowire (NW) networks using chemical etching process. The possible mechanism of the etching phenomenon is discussed. These films were examined for their structural, surface morphological and optical properties by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and UV-vis spectrophotometry techniques, respectively. Photoelectrochemical (PEC) investigations were carried out using cell configuration as n-CdS/(1 M NaOH + 1 M Na₂S + 1 M S)/C. The film of nanowires was found to be hexagonal in structure with the preferential orientation along the (0 0 2) plane. The nanowires have widths in the range of 50-150 nm and have lengths of the order of a few micrometers. Optical studies reveal that the CdS nanowires have value of band gap 2.48 eV, whereas it is 2.58 eV for nanoparticles of CdS. Finally, we report on the ideality of junction improvement of PEC cells when CdS nanoparticles photoelectrode converted into nanowires photoelectrode.     

Preparation and characterization of Mg-doped ZnO thin films by sol-gel method

Undoped and Mg-doped ZnO thin films were deposited on Si(1 0 0) and quartz substrates by the sol-gel method. The thin films were annealed at 873 K for 60 min. Microstructure, surface topography and optical properties of the thin films have been measured by X-ray diffraction (XRD), atomic force microscope (AFM), UV-vis spectrophotometer, and fluorophotometer (FL), respectively. The XRD results show that the polycrystalline with hexagonal wurtzite structure are observed for the ZnO thin film with Mg:Zn = 0.0, 0.02, and 0.04, while a secondary phase of MgO is evolved for the thin film with Mg:Zn = 0.08. The ZnO:Mg-2% thin film exhibits high c-axis preferred orientation. AFM studies reveal that rms roughness of the thin films changes from 7.89 nm to 16.9 nm with increasing Mg concentrations. PL spectra show that the UV-violet emission band around 386-402 nm and the blue emission peak about 460 nm are observed. The optical band gap calculated from absorption spectra and the resistivity of the ZnO thin films increase with increasing Mg concentration. In addition, the effects of Mg concentrations on microstructure, surface topography, PL spectra and electrical properties are discussed.     

Photosensitivity of nanocrystalline ZnO films grown by PLD

We have studied the properties of ZnO thin films grown by laser ablation of ZnO targets on (0 0 0 1) sapphire (Al₂O₃), under substrate temperatures around 400 °C. The films were characterized by different methods including X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and atomic force microscopy (AFM). XPS analysis revealed that the films are oxygen deficient, and XRD analysis with θ-2θ scans and rocking curves indicate that the ZnO thin films are highly c-axis oriented. All the films are ultraviolet (UV) sensitive. Sensitivity is maximum for the films deposited at lower temperature. The films deposited at higher temperatures show crystallite sizes of typically 500 nm, a high dark current and minimum photoresponse. In all films we observe persistent photoconductivity decay. More densely packed crystallites and a faster decay in photocurrent is observed for films deposited at lower temperature.     

Pure UV photoluminescence from ZnO thin film by thermal retardation and using an amorphous SiO2 buffer layer

ZnO/SiO₂ thin films were fabricated on Si substrates by E-beam evaporation with thermal retardation. The as-prepared films were annealed for 2 h every 100 °C in the temperature range 400-800 °C under ambient air. The structural and optical properties were investigated by X-ray diffraction (XRD), atomic force microscopy (AFM) and photoluminescence (PL). The XRD analysis indicated that all ZnO thin films had a highly preferred orientation with the c-axis perpendicular to the substrate. From AFM images (AFM scan size is 1 μm×1 μm), the RMS roughnesses of the films were 3.82, 5.18, 3.65, 3.40 and 13.2 nm, respectively. PL measurements indicated that UV luminescence at only 374 nm was observed for all samples. The optical quality of the ZnO film was increased by thermal retardation and by using an amorphous SiO₂ buffer layer.     

Investigation of thermal annealing effects on microstructural and optical properties of HfO2 thin films

In the present paper, we investigate the effect of thermal annealing on optical and microstructural properties of HfO₂ thin films (from 20 to 190 nm) obtained by plasma ion assisted deposition (PIAD). After deposition, the HfO₂ films were annealed in N₂ ambient for 3 h at 300, 350, 450, 500 and 750 °C. Several characterisation techniques including X-ray reflectometry (XRR), X-ray diffraction (XRD), spectroscopic ellipsometry (SE), UV Raman and FTIR were used for the physical characterisation of the as-deposited and annealed HfO₂ thin films. The results indicate that as-deposited PIAD HfO₂ films are mainly amorphous and a transition to a crystalline phase occurs at a temperature higher than 450 °C depending on the layer thickness. The crystalline grains consist of cubic and monoclinic phases already classified in literature but this work provides the first evidence of amorphous-cubic phase transition at a temperature as low as 500 °C. According to SE, XRR and FTIR results, an increase in the interfacial layer thickness can be observed only for high temperature annealing. The SE results show that the amorphous phase of HfO₂ (in 20 nm thick samples) has an optical bandgap of 5.51 eV. Following its transition to a crystalline phase upon annealing at 750 °C, the optical bandgap increases to 5.85 eV.     

Effects of post-thermal annealing temperature on the optical and structural properties of gold particles on silicon suboxide films

In this work, silicon suboxide (SiO_x) thin films were deposited using a RF magnetron sputtering system. A thin layer of gold (Au) with a thickness of about 10 nm was sputtered onto the surface of the deposited SiO_x films prior to the thermal annealing process at 400 °C, 600 °C, 800 °C and 1000 °C. The optical and structural properties of the samples were studied using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and optical transmission and reflection spectroscopy. SEM analyses demonstrated that the samples annealed at different temperatures produced different Au particle sizes and shapes. SiO_x nanowires were found in the sample annealed at 1000 °C. Au particles induce the crystallinity of SiO_x thin films in the post-thermal annealing process at different temperatures. These annealed samples produced silicon nanocrystallites with sizes of less than 4 nm, and the Au nanocrystallite sizes were in the range of 7-23 nm. With increased annealing temperature, the bond angle of the Si-O bond increased and the optical energy gap of the thin films decreased. The appearance of broad surface plasmon resonance absorption peaks in the region of 590-740 nm was observed due to the inclusion of Au particles in the samples. The results show that the position and intensity of the surface plasmon resonance peaks can be greatly influenced by the size, shape and distribution of Au particles.     

Characteristics of filtered vacuum arc deposited ZnO-SnO2 thin films on room temperature substrates

ZnO, SnO₂ and zinc stannate thin films were deposited using filtered vacuum arc deposition (FVAD) system on commercial microscope glass and UV fused silica substrates (UVFS) at room temperature (RT). The structural and morphological analyses were performed using X-ray diffraction (XRD) and Atomic Force Microscopy (AFM), respectively. XRD patterns of ZnO films deposited at RT had strongly c-axis orientation, whereas SnO₂ and zinc stannate films had amorphous structure as they did not have any defined patterns. Average crystalline size and surface grain size of ZnO films were ∼16 nm, as determined from diffraction line broadening and AFM images, respectively. Optical constants in the 250-1100 nm wavelength range were determined by variable angle spectroscopic ellipsometry and transmission measurements. The transmission of the deposited films in the VIS was 80-90%, affected by interference. The refractive indices and the extinction coefficients of deposited ZnO, SnO₂ and zinc stannate films were in the range 1.87-2.15 and 0.02-0.04, depending on wavelengths and deposition parameters. The optical band gap (E_g) was determined by the dependence of the absorption coefficient on the photon energy at short wavelengths. Its values for ZnO, SnO₂ and zinc stannate were in the range 3.25-3.30 eV, 3.60-3.98 eV and 3.43-3.52 eV, respectively, depending on the deposition pressure.     

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.     

Growth of nanocrystalline CuIn3Se5 (OVC) thin films by ion exchange reactions at room temperature and their characterization as photo-absorbing layers

Nanocrystalline CuIn₃Se₅ thin films have been grown on ITO glass substrates using chemical ion exchange reactions with CdS, in alkaline medium at pH 11. The as-deposited films were annealed in air at 200 °C for 30 min and characterized using X-ray diffraction (XRD), transmission electron microscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, and scanning electron microscopy to study the structural, compositional and morphological properties. The XRD patterns reveal the nanoparticles size to be of 18-20 nm diameter, while from the SEM images the nanoparticles size is estimated to be 20-30 nm. It is observed that the annealed films contain nanocrystallites connected with each other through grain boundaries, with grain size of about 100-125 nm and have an overall n-type electrical conductivity and higher photoconductivity. The current-voltage (I-V) characteristics (in dark and light) of these films indicated the formation of a Schottky like junction between the n-CuIn₃Se₅ (OVC) and CdS/ITO layers.     

Influence of temperature annealing on optical properties of SrTiO3/BaTiO3 multilayered films on indium tin oxide

We have prepared SrTiO₃/BaTiO₃ thin films with multilayered structures deposited on indium tin oxide (ITO) coated glass by a sol-gel deposition and heating at 300-650 °C. The optical properties were obtained by UV-vis spectroscopy. The films show a high transmittance (approximately 85%) in the visible region. The optical band gap of the films is tunable in the 3.64-4.19 eV range by varying the annealing temperature. An abrupt decrease towards the bulk band gap value is observed at annealing temperatures above 600 °C. The multilayered film annealed at 650 ° C exhibited the maximum refractive index of 2.09-1.91 in the 450-750 nm wavelength range. The XRD and AFM results indicate that the films annealed above 600 ° C are substantially more crystalline than the films prepared at lower temperatures which were used to change their optical band gap and complex refractive index to an extent that depended on the annealing temperature.     

Structure and electrical properties of CdIn2O4 thin films prepared by DC reactive magnetron sputtering

CdIn₂O₄ thin films were prepared by direct-current (DC) reactive magnetron sputtering. The structure, surface morphology and the chemical composition of the thin films were analyzed by X-ray diffraction (XRD), atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS), respectively. The electrical properties of the films prepared in different oxygen concentration and annealing treatment were determined, and the effects of the preparing conditions on the structure and electrical properties were also explored. It indicates that the CdIn₂O₄ thin films with uniform and dense surface morphology contain mainly CdIn₂O₄, In₂O₃ phases, and CdO phase is also observed. The XPS analysis confirms the films are in oxygen-deficient state. The electrical properties of these films significantly depend on the preparing conditions, the resistivity of the films with the oxygen concentration of 4.29% is 2.95 × 10⁻⁴ Ω cm and the Hall mobility is as high as 60.32 cm²/V s. Annealing treatment can improve the electrical performance of the films.     

Effect of annealing on properties of electrochemically deposited CdTe thin films

Thin films of CdTe have been deposited onto stainless steel and fluorine-doped tin oxide (FTO)-coated glass substrates from aqueous acidic bath using electrodeposition technique. The different preparative parameters, such as deposition time, bath temperature and pH of the bath have been optimized by photoelectrochemical (PEC) technique to get good quality photosensitive material. The deposited films are annealed at different temperature in presence of air. Annealing temperature is also optimized by PEC technique. The film annealed at 200 °C showed maximum photosensitivity. Different techniques have been used to characterize as deposited and also as annealed (at 200 °C) CdTe thin film. The X-ray diffraction (XRD) analysis showed the polycrystalline nature, and a significant increase in the XRD peak intensities is observed for the CdTe films after annealing. Optical absorption shows the presence of direct transition with band gap energy 1.64 eV and after annealing it decreases to 1.50 eV. Energy dispersive analysis by X-ray (EDAX) study for the as-deposited and annealed films showed nearly stoichiometric compound formation. Scanning electron microscopy (SEM) reveals that spherically shaped grains are more uniformly distributed over the surface of the substrate for the CdTe film.     

Effect of annealing on structural, optical and electrical properties of nanostructured Ge thin films

Ge thin films with a thickness of about 110 nm have been deposited by electron beam evaporation of 99.999% pure Ge powder and annealed in air at 100-500 °C for 2 h. Their optical, electrical and structural properties were studied as a function of annealing temperature. The films are amorphous below an annealing temperature of 400 °C as confirmed by XRD, FESEM and AFM. The films annealed at 400 and 450 °C exhibit X-ray diffraction pattern of Ge with cubic-F structure. The Raman spectrum of the as-deposited film exhibits peak at 298 cm⁻¹, which is left-shifted as compared to that for bulk Ge (i.e. 302 cm⁻¹), indicating nanostructure and quantum confinement in the as-deposited film. The Raman peak shifts further towards lower wavenumbers with annealing temperature. Optical band gap energy of amorphous Ge films changes from 1.1 eV with a substantial increase to ∼1.35 eV on crystallization at 400 and 450 °C and with an abrupt rise to 4.14 eV due to oxidation. The oxidation of Ge has been confirmed by FTIR analysis. The quantum confinement effects cause tailoring of optical band gap energy of Ge thin films making them better absorber of photons for their applications in photo-detectors and solar cells. XRD, FESEM and AFM suggest that the deposited Ge films are composed of nanoparticles in the range of 8-20 nm. The initial surface RMS roughness measured with AFM is 9.56 nm which rises to 12.25 nm with the increase of annealing temperature in the amorphous phase, but reduces to 6.57 nm due to orderedness of the atoms at the surface when crystallization takes place. Electrical resistivity measured as a function of annealing temperature is found to reduce from 460 to 240 Ω-cm in the amorphous phase but drops suddenly to 250 Ω-cm with crystallization at 450 °C. The film shows a steep rise in resistivity to about 22.7 KΩ-cm at 500 °C due to oxidation. RMS roughness and resistivity show almost opposite trends with annealing in the amorphous phase.