In recent decades, the development of organic−inorganic hybrid perovskite solar cells (PSCs) has been increasing very quickly due to their high initial efficiency and low-cost process. However, key points such as crystal growth mechanisms, current−voltage hysteresis, and instability remain still unexplained or misunderstood. Among several possibilities, ionic migration in PSCs has been suggested to explain the hysteresis effect. However, direct experimental evidence of ionic migration under operation or measurement conditions of PSCs is still missing. This work shows directly the ionic migration of halogen components (I − and Cl − ) of a CH 3 NH 3 PbI 3−x Cl x perovskite film under an applied bias using glow discharge optical emission spectrometry (GD-OES). Furthermore, no migration of lead and nitrogen ions is observed on a polarization time scale less than 2 min. The ratio of fixed to mobile iodide ions is deduced from the evolution of the GD-OES profile lines as a function of the applied bias. The average length of iodide and chloride ion migration is deduced from the experimental results.
Ionic migration in halide perovskite materials is now well recognized to affect the electrical properties of perovskite solar cells. Native point defects such as vacancies are considered as responsible for migration of ions. In order to interpret the unusual behavior of current−voltage curves in methylammonium lead tri-iodide perovskite (MAPI) solar cells, we combined two independent experiments: temperaturedependent conductivity measurements (213−363 K) under dark and glow discharge optical emission spectroscopy (GD-OES) under electrical bias conditions. From the film conductivity measurements, we observed two different conduction regimes: an ionic conduction regime at temperatures higher than 263 K, associated with an activation energy of 0.25 eV, and an electronic conduction regime below 263 K. At room temperature, both conductivities are around 10 −7 S/cm. From GD-OES, we observed directly a reversible migration of iodide ions under positive or negative bias (minute time scale) at room temperature and deduced an iodide ion diffusion coefficient of 1.3 × 10 −12 cm 2 •s −1 and a mobility of 5 × 10 −11 cm 2 •V −1 •s −1 .
The aim of the paper is to study and determine the effect of voltage increasing from 500 up to 650 V DC on chemical and electrochemical properties of the obtained porous coatings with plasma electrolytic oxidation (PEO) processes, known also as micro arc oxidation (MAO). In the present paper, the chemical and electrochemical characterization of porous phosphate coatings enriched with magnesium or zinc on commercially pure (CP) Titanium Grade 2 under DC-PEO obtained in electrolytes based on concentrated 85% analytically pure H 3 PO 4 (98 g/mole) acid with additions of 500 g•L −1 of zinc nitrate Zn(NO 3) 2 •6H 2 O or magnesium nitrate Mg(NO 3) 2 •6H 2 O, are described. These materials were characterized using scanning electron microscope (SEM) with energy-dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and glow discharge optical emission spectroscopy (GDOES). It was found that the voltage of PEO process has influence on the chemical composition and thickness of the obtained porous coatings as well as on their electrochemical behavior. The higher the potential of PEO treatment, the higher the amount of zinc-to-phosphorus ratio for zinc enriched coatings was obtained, whereas in magnesium enriched coatings, the average amount of magnesium detected in PEO coating is approximately independent of the PEO voltages. Based on XPS studies, it was found out that most likely the top 10 nm of porous coatings is constructed of titanium (Ti 4+), magnesium (Mg 2+), zinc (Zn 2+), and phosphates PO 4 3− and/or HPO 4 2− and/or H 2 PO 4 − and/or P 2 O 7 4−. On the basis of GDOES studies, a four-sub-layer model of PEO coatings is proposed. Analysis of the potentiodynamic corrosion curves allowed to conclude that the best electrochemical repeatability was noted for magnesium and zinc enriched coatings obtained at 575 V DC .
Antibacterial cerium-doped hydroxyapatite (Ce-HAp) layers have been researched sparingly in recent years. The Ce-HAp powder, Ca10−xCex(PO4)6(OH)2 with xCe = 0.05, was obtained by an adapted chemical co-precipitation method at room temperature. The target was prepared using the Ce-HAp (xCe = 0.05) powder sintered in air at 600 °C. The coatings on the Ti substrate were generated in plasma using a radio frequency (RF) magnetron sputtering discharge in an Ar gas flow in a single run. To collect the most complete information regarding the antimicrobial activity of cerium-doped hydroxyapatite with xCe = 0.05, (5Ce-HAp), antimicrobial studies were carried out both on the final suspensions and on the coated surfaces. The target was tested using ultrasound measurement, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), glow-discharge optical emission spectroscopy (GDOES), and X-ray photoelectron spectroscopy (XPS). The present study exhibited for the first time results of the homogeneous coatings of hydroxyapatite doped with cerium using a radio frequency magnetron sputtering technique. In addition, this study highlighted for the first time the stability of the cerium-doped hydroxyapatite gels used in the creation of the coating. Ultrasound measurements on the concentrated suspension of 5Ce-HAp showed a good stability compared to double distilled, water which was chosen as the reference fluid. Particles with spherical shape were observed by both TEM and SEM analysis. The broadening of the IR bands in the IR spectrum of the 5Ce-HAp film in comparison with the IR spectrum of the precursor target indicate the formation of interlinked bonds into the layer bulk. XPS analysis revealed that the mixture of Ce3+ and Ce4+ ions in the hydroxyapatite (HAp) structure of the coatings could be due to the deposition process. The surface of 5Ce-HAp coatings was homogenous with particles having a spherical shape. A uniform distribution of all the constituent elements on the surface the 5Ce-HAp layer was revealed. The antimicrobial assays proved that both 5Ce-HAp suspensions and 5Ce-HAp coatings effectively inhibited the development of colony forming units (CFU) for all the tested microbial strains. Moreover, the antimicrobial assays emphasized that the 5Ce-HAp suspensions had a biocide effect against Escherichia coli (E. coli) and Candida albicans (C. albicans) microbial strains after 72 h of incubation.
Abstract:In the paper, Scanning Electron Microscopy (SEM), Energy-dispersive X-ray Spectroscopy (EDS), X-ray Photoelectron Spectroscopy (XPS), and Glow Discharge Optical Emission Spectroscopy (GDOES) analyses of calcium-and phosphorus-enriched coatings obtained on commercial purity (CP) Titanium Grade 2 by plasma electrolytic oxidation (PEO), known also as micro arc oxidation (MAO), in electrolytes based on concentrated phosphoric acid with calcium nitrate tetrahydrate, are presented. The preliminary studies were performed in electrolytes containing 10, 300, and 600 g/L of calcium nitrate tetrahydrate, whereas for the main research the solution contained 500 g/L of the same hydrated salt. It was found that non-porous coatings, with very small amounts of calcium and phosphorus in them, were formed in the solution with 10 g/L Ca(NO 3 ) 2 ·4H 2 O, whereas the other coatings, fabricated in the consecutive electrolytes containing from 300 up to 650 g/L Ca(NO 3 ) 2 ·4H 2 O, were porous. Based on the GDOES data, it was also found that the obtained porous PEO coating may be divided into three sub-layers: the first, top, porous layer was the thinnest; the second, semi-porous layer was about 12 times thicker than the first; and the third, transition sub-layer was about 10 times thicker than the first. Based on the recorded XPS spectra, it was possible to state that the top 10-nm layer of porous PEO coatings included chemical compounds containing titanium (Ti 4+ ), calcium (Ca 2+ ), as well as phosphorus and oxygen (PO 4 3− and/or HPO 4 2− and/or H 2 PO 4 − , and/or P 2 O 7 4− ).
The goal of this paper was to investigate the antifungal activity of Enamel layers deposited on titanium substrate (Ti-Enamel) and Enamel layers deposited on titanium substrate previously coated with a vinyl polydimethylsiloxane layer (Ti-PDMS-Enamel). The physicochemical properties were also investigated. TheCandida albicansbiofilm development on the obtained layers was examined after 24 h, 48 h, and 72 h by confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM) after ethidium bromide staining. A significant inhibition of the fungal adherence and biofilm development was observed on Ti-Enamel layers. The antifungal results demonstrated that the use of new Ti-Enamel composite layers could represent a promising perspective for the prevention of fungal biofilms associated implant infections.
Post-implant infections are a major health problem, and it is well-known that treating them with conventional drugs is accompanied by many disadvantages. The development of new biomaterials with enhanced antimicrobial properties are of major interest for the scientific world. The aim of this study was to synthesize and characterize hydroxyapatite doped with Samarium (Ca10−xSmx(PO4)6(OH)2, xSm = 0.05, 5Sm-HAp) suspensions, pellets and coatings. The 5Sm-HAp coatings on Si substrates were obtained by rf magnetron sputtering technique. The different techniques such as ultrasound measurements, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Glow Discharge Optical Emission Spectroscopy (GDOES), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) were used to examine the obtained coatings. The results showed that the doped Sm ions entered the structure of hydroxyapatite successfully and Sm ions was uniformly doped onto the surface of the support. The depth profile curves of Ca, P, O, H, Ce and Si elements exhibit their presence from a surface to substrate interface as function of sputtering time. XPS analysis indicated as calcium-phosphate structures enriched in Sm3+ ions. Furthermore, the antimicrobial properties of the 5Sm-HAp suspensions, targets and coatings were assessed against Escherichia coli ATCC 25922, Staphylococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results of the antimicrobial assays highlighted that that the samples presented a strong antimicrobial activity against the tested microbial strains. The results showed that the coatings after 48 h of incubation inhibited the growth of all tested microbial strains under the value of 0.6 Log CFU/mL. This study shows that the 5Sm-HAp samples are good candidates for the development of new antimicrobial agents.
Bilayer VO2 films made using ElFi-AACVD and sol–gel spin coating with ZnO, SnO2 or WO3 top-layers show superior thermochromic properties.
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