Characterization of poly(vinyl chloride) powder produced by emulsion polymerization

The effect of emulsion process formulation ingredients on the morphology, structure, and properties of polyvinyl chloride (PVC) powder has been considered in this study. PVC powder was extracted with ethanol and films were obtained by solvent casting from tetrahydrofurane. Characterization of powders, films, and ethanol extract was performed through FTIR spectroscopy, DSC, AFM, SEM, EDX analysis, methylene blue, and nitrogen adsorption. PVC powder was composed of spheres of a large particle size range from 10 nm to 20 μm as shown by SEM. The specific surface area of the PVC powder was determined as 16 and 12 m² g⁻¹ from methylene blue adsorption at 25 °C and from N₂ adsorption at −196 °C, respectively. AFM indicated the surface roughness of the films obtained by pressing the particles was 25.9 nm. Density of PVC powder was determined by helium pycnometry as 1.39 g cm⁻³. FTIR spectroscopy indicated that it contained carbonyl and carboxylate groups belonging to additives such as surface active agents, plasticizers, and antioxidants used in production of PVC. These additives were 1.6% in mass of PVC as determined by ethanol extraction. EDX analysis showed PVC particles surfaces were coated with carbon-rich materials. The coatings had plasticizer effect since, glass transition temperature was lower than 25 °C for PVC powder and it was 80 °C for ethanol extracted powders as found by using differential scanning calorimetry. These additives from polymerization process made PVC powder more thermally stable as understood from Metrom PVC thermomat tests as well.     

Structure and multiferroic properties of Bi<Subscript>5</Subscript>FeTi<Subscript>3</Subscript>O<Subscript>15</Subscript> thin films prepared by the sol–gel method

The Bi₅FeTi₃O₁₅ (BFTO) films of layered structure have been fabricated on Pt/Ti/SiO₂/Si substrates by the sol–gel method. The thermal decomposition behaviors of precursor powder were examined using thermo-gravimetric and differential scanning calorimeters analysis. The optimal heat treatment process for BFTO films were determined to be low-temperature drying at 200 °C for 4 min and high-temperature drying at 350 °C for 5 min followed by annealing at 740 °C for 60 min, which led to the formation of compact films with uniform grains of ~300 nm. The structural, surface topography, ferroelectric and magnetic properties of the films were investigated. The remnant polarization (2P _r) of BFTO thin films under an applied electric field of ~550 kV/cm are determined to be 67.5 μC/cm² . Meanwhile, the weak ferromagnetic properties of the BFTO films were observed at room temperature.     

Fabrications of Nb-doped TiO<Subscript>2</Subscript> (TNO) transparent conductive oxide polycrystalline films on glass substrates by sol–gel method

Anatase Ti_0.94Nb_0.06O₂ (TNO) films were fabricated on glass substrates by sol–gel method using a dip-coating technique. The annealing treatment was separated into two steps, first in air at 350–550 °C for 1 h and then in vacuum of 4.0 × 10⁻⁴ Pa at 550 °C for 1 h. The influence of vacuum annealing treatment to the electrical and optical properties was discussed. Especially, the role of air annealing treatment from 350 to 550 °C on the crystallization and the structure of the films was analyzed. It is proved that the films annealed at 550 °C in air and then 550 °C in vacuum exhibited the minimum resistivity of 19.3 Ω·cm and the average optical transmittance of about 75% in the visible range, indicating that the sol–gel method is a feasible and promising method to fabricate TNO films.     

Optically transparent superhydrophobic TEOS-derived silica films by surface silylation method

Optically transparent silica films were prepared at room temperature (~27°C) by keeping the molar ratio of TEOS:MeOH:H₂O (0.001 M NH₄F) constant at 1:19.29:6.20, respectively. A surface chemical modification of the films was done with alkylchlorosilanes at different concentrations from 0 to 1 vol. % and aging times varied from half to 2 h. The DMCS and TMCS surface modified silica films showed the static water contact angle of 146° and 162°, respectively. When the DMCS and TMCS modified films were cured at temperatures higher than 240 and 275°C, respectively, the films became superhydrophilic. Further, the humidity study was carried out at a relative humidity of 90% at 30°C temperature over 60 days. We characterized the water repellent silica films by Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy, % of optical transmission, humidity tests and contact angle measurements.     

Preparation and phase transition characterization of VO2 thin film on single crystal Si (100) substrate by sol–gel process

Vanadium dioxide (VO₂) thin films were fabricated on single crystal Si (100) substrates by sol–gel method, including a process of annealing a vanadium pentoxide (V₂O₅) gel precursor at different temperatures. The crystalline structure and morphology of the films were investigated by XRD, FE-SEM and AFM, indicating that the films underwent the grain growth, agglomeration and grain refinement process with increased annealing temperatures. The film annealed at 500 °C exhibits the formation of VO₂ phase with a strong (011) preferred orientation and high crystallinity, the surface of the film is uniform and compact with a grain size of about 120 nm. Meanwhile, the film exhibits excellent phase transition properties, with a decrease of transmittance from 35.5 to 2.5% at λ = 25 μm and more than 3 orders of resistivity magnitude variation bellow and above the phase transition temperature. The phase transition temperature is evaluated at 60.4 °C in the heating transition and 55.8 °C in the cooling transition. Furthermore, the phase transition property of the VO₂ film appears to be able to remain stable over repetitive cycles 100 times.     

Preparation and characterization of transparent TiO2 thin films coated on fused-silica substrates

The transparent TiO₂ thin films coated on fused-SiO₂ substrates were prepared by the sol–gel method and spin-coating technique. Effects of calcination temperature on crystal structure, grain size, surface texture, and light transmittance of the films were investigated. After calcining at 600–1,200 °C, the thicknesses of the TiO₂ films were all around 80 nm and the molecular structures of the films were anatase, even at 1,200 °C. The calcined TiO₂ films had the ultraviolet light (wavelength 200–400 nm) transmittances of ≤29% and the visible light (wavelength 400–800 nm) transmittance of ≥72%. By photocatalytically decomposing the methylene blue (MB) in water, the photocatalytic activities of the TiO₂ thin films were measured and represented using the characteristic time constant (τ) for the MB degradation. While the films prepared at 1,000 and 1,200 °C photodecomposed about 54 mol% of the MB in water (the corresponding τ ≈ 14.8 h) after exposing to 365-nm UV light for 12 h, the films prepared at 600 and 800 °C had smaller τ (≈9.0 h) and photodecomposed about 74 mol% of the MB in water at the same testing conditions.     

Study of the morphology,thermal and mechanical properties of irradiated isotactic polypropylene films

Thin films of isotactic polypropylene (iPP) are of great economical importance and their production is quite challenging due to the need of very fast uniaxial or biaxial expansion. During the expansion, critical problems usually arise, like structure disruption, shear thinning, causing material, energy and time losses. This work aims to study the surface morphology and compare the thermal, mechanical properties of PP films irradiated by gamma ray in an acetylene atmosphere after uniaxial expansion. PP films were made by compression molding at 190 °C with cooling in water at room temperature and irradiated by gamma ray, at (5, 12.5 and 20 kGy) under acetylene atmosphere. After irradiation the samples were submitted to thermal treatment at 90 °C for 1 h and then stretched out at 170 °C using an Instron machine. The surface of PP films, pristine and modified, (i.e., irradiated), was studied using optical microscopy (OM) and scanning electron microscopy (SEM). The changes in morphology, crystallinity and tensile parameters, like yield stress, rupture stress and elongation strain of the PP with irradiation dose were investigated. The results showed some evidences of gel formation due to crosslinking and/or long chain branching induced by radiation.     

Modifying transparent electrode with conjugated organic semiconductor hole transport material as interface for enhancing performance of organic solar cell

Indium tin oxide (ITO) is used as a substrate was covered with 4-[4-(4-methoxy-N-naphthalen-2-ylanilino) phenyl] benzoic acid (MNA) as a self-assembled monolayer (SAM). Poly(3-hexylthiophene) (P3HT) and 1-(3-methoxycarbonyl)-propyl-1-phenyl-(6,6) C₆₁ (PCBM) were mixed and used as a donor–acceptor in organic solar cell (OSC). The MNA (SAM) layer is used as an interface instead of poly(3,4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT: PSS) for hole injection. The HOMO-LUMO energy level of MNA-SAM molecule and the electronic charge distribution were calculated theoretically using Chemissian software. The HOMO-LUMO energy level of the MNA is calculated as E_HOMO = ?5.10 eV and E_LUMO = ?1.60 eV. The OSC modified with MNA showed an efficient performance in the absence of PEDOT: PSS as hole transport layer. The annealing of the ITO/SAM/P3HT: PCBM films at different temperatures are also investigated to study the effect of reducing defects. The interface structures of the organic semiconductor layer on ITO were characterized by Atomic Force Microcopy (AFM). In addition, Kelvin Probe Microscopy (KPM) is used to understand how the annealing changes the surface potential energy of the ITO/SAM substrate. Using the KPM method, which measures the surface potential energy of the films, the energy bands of the ITO were increased to maximum 5.09 eV. The ITO/SAM/P3HT: PCBM film's surface potential was determined to be 0.18 eV after being annealed at 80 °C. The surface potential of the modified films was discovered to be 0.33 V and 0.39 V when the annealing temperature was raised from 80 °C to 120 °C and 160 °C. The maximum device efficiency was demonstrated by the ITO/SAM/P3HT: PCBM film after an hour of annealing at 160 °C.     

The effect of different substrate temperatures on the structure and luminescence properties of Y2O3:Bi3+ thin films

Y₂O₃:Bi³⁺ phosphor thin films were prepared by pulsed laser deposition in the presence of oxygen (O₂) gas. The microstructure and photoluminescence (PL) of these films were found to be highly dependent on the substrate temperature. X-ray diffraction analysis showed that the Y₂O₃:Bi³⁺ films transformed from amorphous to cubic and monoclinic phases when the substrate temperature was increased up to 600 °C. At the higher substrate temperature of 600 °C, the cubic phase became dominant. The crystallinity of the thin films, therefore, increased with increasing substrate temperatures. Surface morphology results obtained by atomic force microscopy showed a decrease in the surface roughness with an increase in substrate temperature. The increase in the PL intensities was attributed to the crystallinity improvement and surface roughness decrease. The main PL emission peak position of the thin films prepared at substrate temperatures of 450 °C and 600 °C showed a shift to shorter wavelengths of 460 and 480 nm respectively, if compared to the main PL peak position of the powder at 495 nm. The shift was attributed to a different Bi³⁺ ion environment in the monoclinic and cubic phases.     

Evolution of crystalline structure in SnS thin films prepared by chemical deposition

Crystal structure and morphology undergo significant evolution in thin films of tin(II) sulfide prepared by chemical deposition, over a narrow interval of bath temperature of 20–40 °C, but has not been recognized in previous studies. The chemical bath is constituted using tin(II) chloride, triethanolamine, ammonia(aq.) and thioacetamide. At bath temperature of 20 °C, the deposition rate of the film is 10 nm/h; and at 24 h, a film of thickness 260 nm is obtained. This film is compact and with a predominantly cubic (Cub-) crystalline structure. At 40 °C, the deposition rate is 25 nm/h, and a film of 600 nm in thickness is deposited in 24 h. However, this film has evolved into vertically stacked platelets of orthorhombic (OR-) crystalline structure. The transition from compact-to-platelet morphology as well as from Cub-to-OR-crystalline structure is observed near a deposition temperature, 35 °C. The Cub-SnS has a characteristic high optical band gap, 1.67 eV (direct gap; forbidden transitions) with an electrical conductivity, 10⁻⁷(Ω cm)⁻¹; both properties being un-affected when films are heated at 300 °C in a nitrogen ambient. In OR-SnS, the band gap is 1.1 eV (indirect gap; allowed transitions). The electrical conductivity of such films is notably higher, 10⁻⁴ (Ω cm)⁻¹, which increases further by an order of magnitude when the films have been heated at 300 °C in nitrogen.     

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.     

The influence of precursor temperature on strontium sulphide doped silver for optoelectronic application

This research aims at the study of strontium sulphide doped silver using 0.1 mol of strontium chloride hexahydrate (SrCl2.6H2O), Thioacetamide (C₂H₅NS), and 0.01 mol of silver nitrate (AgNO3) as the cationic, anionic, and dopant concentrations via electrochemical deposition technique. The film had a strong peak at (111) and (211) which corresponds to 2theta values of 26.69° and 51.77° for undoped SrS and doped SrS respectively, and a flawless crystalline peak with a cubic phase that is indexed at orientations (111), (112), (200), and (211). SrS/Ag of deposited different precursor temperatures (room, 35, 40, and 45)^o correspond to 2theta values of 26.69°, 33.79°, 37.60°, and 51.77° respectively. The crystal lattice is shown by the rise in peak intensity with higher 2theta degree values; the appearance of an unindexed peak is caused by the substrate utilized for the deposition. Clove-like material with precipitate is visible in the SrS material's micrograph; the big nano grain on the surface of the substrate exhibits photon absorption but lacks any signs of pinholes. At the introduction of dopant and heating the precursor at 35 °C, 40 °C, and 45 °C there is a drastic change in the micrograph of the films, for the films at 35 °C the nanoparticle clave together with a melted wax with a sharp large white precipitate which is very visible on the surface of the film and the material deposited at 40 °C and 45 °C there is no visible precipitate on the film which show that as the precursor temperature increases it eliminate lattice strain and improve the photovoltaic properties of the deposited material. The energy band gap of strontium sulphide (SrS) and strontium sulphide doped silver (SrS/Ag) at different precursor temperatures of 35 °C, 40 °C, 45 °C is 1.50–2.35 eV.     

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.     

Mesoporous and nanocrystalline sol–gel derived NiTiO3 at the low temperature: Controlling the structure,size and surface area by Ni:Ti molar ratio

Nanocrystalline nickel titanate (NiTiO₃) thin films and powders with mesoporous structure were produced at the low temperature of 500 °C by a straightforward particulate sol–gel route. The sols were prepared in various Ni:Ti molar ratios. X-ray diffraction and Fourier transform infrared spectroscopy revealed that the powders contained mixtures of the NiTiO₃ and NiO phases, as well as the anatase-TiO₂ and the rutile-TiO₂ depending on the annealing temperature and Ni:Ti molar ratio. Moreover, it was found that Ni:Ti molar ratio influences the preferable orientation growth of the nickel titanate, being on (202) planes for the nickel dominant powders (Ni:Ti ≥ 75:25) and on (104) planes for the rest of the powders (Ni:Ti: ≤ 50:50). The average crystallite size of the powders annealed at 500 °C was in the range 1.5–2.4 nm and a gradual increase occurred up to 8 nm by heat treatment at 800 °C. The activation energy of crystal growth decreased with an increase of Ni:Ti molar ratio, calculated in the range 24.93–37.17 kJ/mol. Field emission scanning electron microscope analysis revealed that the deposited thin films had mesoporous and nanocrystalline structure with the average grain size of 20–35 nm. Moreover, atomic force microscope images presented that the thin films had a hill-valley like morphology with roughness mean square in the range 41–57 nm. Based on Brunauer–Emmett–Taylor analysis, the synthesized powders showed mesoporous structure containing pores with needle and plate like shapes. The mesoporous structure of the powders was stable at high annealing temperatures and one of the highest surface areas (i.e., 156 m²/g) reported in the literature was obtained for the powder containing Ni:Ti = 50:50 at 500 °C.     

Properties of cellulose films prepared from NaOH/urea/zincate aqueous solution at low temperature

Cellulose films were successfully prepared from NaOH/urea/zincate aqueous solution pre-cooled to −13 °C by coagulating with 5% H₂SO₄. The cellulose solution and regenerated cellulose films were characterized with dynamic rheology, ultraviolet–visible spectroscope, scanning electron microscopy, wide angle X-ray diffraction, Fourier transform infrared (FT-IR) spectrometer, thermogravimetry and tensile testing. The results indicated that at higher temperature (above 65 °C) or lower temperature (below −10 °C) or for longer storage time, gels could form in the cellulose dope. However, the cellulose solution remained a liquid state for a long time at 0–10 °C. Moreover, there was an irreversible gelation in the cellulose solution system. The films with cellulose II exhibited better optical transmittance, high thermal stability and tensile strength than that prepared by NaOH/urea aqueous solution without zincate. Therefore, the addition of zincate in the NaOH/urea aqueous system could enhance the cellulose solubility and improve the structure and properties of the regenerated cellulose films.     

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.     

Electric-field-induced antiferroelectric to ferroelectric and ferroelectric to paraelectric phase transition at various temperatures in (Pb,La)(Zr,Ti)O<Subscript>3</Subscript> antiferroelectric thick films

(Pb, La)(Zr, Ti)O₃ antiferroelectric thick films with (100)-preferred orientation were fabricated on Pt(111)/Ti/SiO₂/Si(100) substrates via a sol–gel method. The electric-field-induced antiferroelectric (AFE) to ferroelectric (FE) phase transition characteristics were studied by C (capacitance)–E (electric field) measurements at different temperature. The films were in AFE state under 0 kV/cm below 122 °C, and the switching field values decreased, with increasing temperature. The films were in FE state between 122 and 135 °C, and when the temperature above 135 °C, the films were in PE state. The temperature-dependent dielectric parameters were deconvoluted using a Gaussian fit multi-peaks showed that two typical phase transitions were discovered. The first peak is the AFE-to-FE phase transition and the second peak is the FE-to-PE phase transition which has been verified by C–E tests.     

Cu-particle-dispersed (K<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)NbO<Subscript>3</Subscript> composite thin films derived from sol–gel processing

Sol–gel processing of Cu-particle-dispersed (K_0.5Na_0.5)NbO₃ (Cu/KNN) thin films was studied in an attempt to develop a method producing piezoelectric composite films with good mechanical performance. The Cu/KNN films were prepared via crystallization annealing at 650–750 °C for 1 min in air, followed by reduction annealing at 400–500 °C for 1–2 h in a 5% H₂ and 95% Ar gas mixture. The resultant composite films consisted of perovskite KNN, metallic Cu, and Cu₄O₃. This suggests that the decomposition of Cu sources takes two different ways in this study. The Cu/KNN composite films containing Cu₄O₃ phases were produced by the crystallization annealing at 700 °C for 1 min followed by the reduction annealing at 500 °C for 1 h. Surface morphology observations reveal that these films have dense KNN matrix with a grain size of ~200 nm and uniformly dispersed Cu or Cu₄O₃ particles with a size of <500 nm.     

Microstructure,dielectric properties and optical band gap control on the photoluminescence behavior of Ba[Zr<Subscript>0.25</Subscript>Ti<Subscript>0.75</Subscript>]O<Subscript>3</Subscript> thin films

Ba[Zr_0.25Ti_0.75]O₃ (BZT) thin films were synthesized by the complex polymerization method and heat treated at 400 °C for different times and at 700 °C for 2 h. These thin films were analyzed by X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, field emission gun-scanning electron microscopy (FEG-SEM) and atomic force microscopy (AFM), Ultraviolet–visible (UV–vis) absorption spectroscopy, electrical and photoluminescence (PL) measurements. FEG-SEM and AFM micrographs showed that the microstructure and thickness of BZT thin films can be influenced by the processing times. Dielectric constant and dielectric loss of BZT thin films heat treated at 700 °C were approximately 148 and 0.08 at 1 MHz, respectively. UV–vis absorption spectra suggested the presence of intermediary energy levels (shallow and deep holes) within the band gap of BZT thin films. PL behavior was explained through the optical band gap values associated to the visible light emission components.     

An investigation of the microstructure,optical and electrical properties of ZITO thin film using the sol–gel method

The multi-compound ZITO transparent conductive oxide (TCO) thin films were synthesized using the sol–gel method. The ZITO thin films with various volume ratios of ZnO to ITO (1:1, 2:1 and 9:1) were crystallized at different temperatures (600–700 °C). The results showed that the crystalline characteristics and optical transmittance were mainly dependent on ITO content and crystallization. Notably, the 650 °C Z₉ITO film not only had better conductivity but also possessed excellent optical transmittance. In addition, the surface roughness of the ZITO films and optoelectric properties of IZO (indium doped ZnO) films were analyzed to confirm the contribution of indium dopants on the optical transmittance. Also, the ZITO films were subjected to the effects of indium and tin dopants and this improved the related characteristics of ZnO films.