Search Results (17)

This study focuses on the deposition of fullerene (C₆₀) as thin film on glass substrate by ultrasonic chemical bath deposition (UCBD) processing, under ambient temperature. Highly effective results were obtained from the films based on the solution of C₆₀ dissolved in toluene mixed with 2-methoxyethanol. The obtained films were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). The XRD examination of the thin films reveals the presence of the C₆₀ cubic phase compared to the powder reference. The molecular structure obtained by Rietveld refinement shows no bonding between the molecules in C₆₀ powder, while in the deposed thin film the bonding is established. The molecules are bonded between them by pentagons of the right and left molecule. Each four neighbor molecules bond between them and they are all able to geometrically tie to the neighboring molecules under a crystalline FCC structure. The Sherrer and W-H methods were used to investigate microstructural parameters. The lattice parameter and the crystallite size show the same variation tendency. The average lattice parameter for the powder and the deposed films C₆₀-3h, C₆₀-5h, and C₆₀-8h is 14.0652, 14.1901, 14.0529, and 14.1848 Å, respectively, and the crystallite size calculated by the Sherrer method is 37.51, 38.98, 34.35, and 41.54 nm, respectively, as well. The IR spectrum indicated the presence of chemical π bonds (c=c) that are very suitable for enhancing the electronic properties of the material, and SEM analysis illustrated a dense, homogeneous without pinhole structures in the film morphology. Moreover, EDS emphasizes the presence of high carbon concentration and fewer stranger atoms. As a result, despite the UCBD technique being old and not very often applied in the field of organic materials, it is still a cost effective and good alternative method for organic thin film deposition. Full article

Strontium aluminate, with suitable lattice parameters and environmentally friendly water solubility, has been strongly sought for use as a sacrificial layer in the preparation of freestanding perovskite oxide thin films in recent years. However, due to this material’s inherent water solubility, the methods used for the preparation of epitaxial films have mainly been limited to high-vacuum techniques, which greatly limits these films’ development. In this study, we prepared freestanding single-crystal perovskite oxide thin films on strontium aluminate using a simple, easy-to-develop, and low-cost chemical full-solution deposition technique. We demonstrate that a reasonable choice of solvent molecules can effectively reduce the damage to the strontium aluminate layer, allowing successful epitaxy of perovskite oxide thin films, such as 2-methoxyethanol and acetic acid. Molecular dynamics simulations further demonstrated that this is because of their stronger adsorption capacity on the strontium aluminate surface, which enables them to form an effective protective layer to inhibit the hydration reaction of strontium aluminate. Moreover, the freestanding film can still maintain stable ferroelectricity after release from the substrate, which provides an idea for the development of single-crystal perovskite oxide films and creates an opportunity for their development in the field of flexible electronic devices. Full article

The anthropogenic impact on the environment has long been known to negatively affect the quality of air. Volatile organic compounds (VOCs) are widely used in domestic and industrial applications, generally as solvents. They are mobile in both gaseous and aqueous phases, and thus their spread in environment could have massive effect with dramatically negative consequences. Pulsed corona discharge (PCD) and photocatalytic oxidation (PCO) are considered as efficient and eco-friendly methods for the energy-efficient abatement of gaseous hazardous pollutants. One of the main problems of PCD application in air treatment, however, is residual ozone, a side product of air ionization considered as secondary air pollution. Photocatalytic processes are known to degrade ozone extending simultaneously the photocatalyst lifetime. Thus, combining PCD and PCO in a two-step treatment system could solve the problem of the presence of residual ozone and complement each other’s strengths. In this study, experiments were conducted in separate systems, i.e. photocatalysis and plasma, making a prerequisite for the progress in the combined PCD/PCO applications. A prototype PCO reactor was built and tested with ozone and 2-methoxyethanol (2ME) in combinations. 2ME was chosen as a hazardous model VOC used in industry in solvents and paints. For the PCD experiments xylene was tested. Being refractory air pollutant, extensively studied for its removal, xylene provides a basis for the comparison of its abatement methods. The PCD treatment showed unequalled energy efficiencies in gaseous xylene oxidation. With respect to PCO experiments, the degradation of 2ME and ozone was 40% and 95%, respectively. High ozone degradation performed by PCO confirms the expediency of proposed air cleaning combination. Full article

Ionic liquids have been the subject of intense research because of their unique electrochemical properties and potential applications in various fields. In this article, we analyze the electrical conductivity of two selected ionic liquids, 1-hexyl-3-methylimidazolium chloride (HMIM) and 1-eethyl-3-octylimidazolium chloride (OMIM), in various alkoxy alcohols such as 2-methoxyethanol, 2-ethoxyethanol, 2-propoxyethanol and 2-butoxyethanol. Our research focuses on attempting to analyze the impact of the molecular structure of both the ionic liquids and alkoxy alcohols on their electrical conductivity properties. The results of our study can be highly beneficial in the design of advanced electrochemical materials and their various applications. Full article

Here we present comparative studies of: (i) the formation of ZnO thin films via the sol-gel method using zinc acetate dihydrate (ZAD), 2-methoxyethanol (ME) as solvent, and the aminoalcohols (AA): ethanolamine, (S)-(+)-2-amino-1-propanol, (S)-(+)-2-amino-3-methyl-1-butanol, 2-aminophenol, and aminobenzyl alcohol, and (ii) elemental analyses, infrared spectroscopy, X-ray diffraction, scanning electron microscopy, absorption and emission spectra of films obtained after deposition by drop coating on glass surface, and thermal treatments at 300, 400, 500 and 600 °C. The results obtained provide conclusive evidences of the influence of the AA used (aliphatic vs. aromatic) on the ink stability (prior to deposition), and on the composition, structures, morphologies, and properties of films after calcination, in particular, those due to the different substituents, H, Me, or ⁱPr, and to the presence or the absence of a –CH₂ unit. Aliphatic films, more stable and purer than aromatic ones, contained the ZnO wurtzite form for all annealing temperatures, while the cubic sphalerite (zinc-blende) form was also detected after using aromatic AAs. Films having frayed fibers or quartered layers or uniform yarns evolved to “neuron-like” patterns. UV and photoluminescence studies revealed that these AAs also affect the optical band gap, the structural defects, and photo-optical properties of the films. Full article

The aim of the study is to investigate the influence of the solvents applied both in sol–gel process and for supercritical drying (SCD) on NiO aerogels’ properties. NiO aerogels were synthesized using methanol and 2-methoxy-ethanol (MeGl) as sol solvents. SCD was performed using iso-propanol, methanol and tert-butyl-methyl ether as supercritical fluids. The obtained samples were characterized using low-temperature nitrogen adsorption, X-ray diffraction analysis, mass-spectra analysis and STEM and TEM methods. It was found that specific surface area and the phase and chemical composition strongly depend on the synthesis conditions. We revealed that Ni²⁺ cations were reduced into Ni⁰ when 2-methoxy-ethanol was applied as a sol solvent. The mechanism of the Ni²⁺ cations reduction is proposed. We consider that at the stage of sol preparation, the Ni²⁺–MeGl chelate was formed. This chelate decomposes at the SCD stage with the release of MeGl, which, in turn, eliminates methanol and leads to the formation of aldehyde. The latter is responsible for the nickel reduction. The proposed mechanism was confirmed experimentally. Full article

The present study is focused on the synthesis of zirconium dioxide (ZrO₂) nanomaterials using the hydrothermal method assisted by microwave irradiation and solution combustion synthesis. Both synthesis techniques resulted in ZrO₂ powders with a mixture of tetragonal and monoclinic phases. For microwave synthesis, a further calcination treatment at 800 °C for 15 min was carried out to produce nanopowders with a dominant monoclinic ZrO₂ phase, as attested by X-ray diffraction (XRD) and Raman spectroscopy. The thermal behavior of the ZrO₂ nanopowder was investigated by in situ XRD measurements. From the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images, the presence of near spherical nanoparticles was clear, and TEM confirmed the ZrO₂ phases that comprised the calcinated nanopowders, which include a residual tetragonal phase. The optical properties of these ZrO₂ nanopowders were assessed through photoluminescence (PL) and PL excitation (PLE) at room temperature (RT), revealing the presence of a broad emission band peaked in the visible spectral region, which suffers a redshift in its peak position, as well as intensity enhancement, after the calcination treatment. The powder resultant from the solution combustion synthesis was composed of plate-like structures with a micrometer size; however, ZrO₂ nanoparticles with different shapes were also observed. Thin films were also produced by solution combustion synthesis and deposited on silicon substrates to produce energy storage devices, i.e., ZrO₂ capacitors. The capacitors that were prepared from a 0.2 M zirconium nitrate-based precursor solution in 2-methoxyethanol and annealed at 350 °C exhibited an average dielectric constant (κ) of 11 ± 0.5 and low leakage current density of 3.9 ± 1.1 × 10⁻⁷ A/cm² at 1 MV/cm. This study demonstrates the simple and cost-effective aspects of both synthesis routes to produce ZrO₂ nanomaterials that can be applied to energy storage devices, such as capacitors. Full article

In this work, the synthesis of ordered mesoporous silica of MCM-41 type was investigated aimed at improving its morphology by varying the synthesis conditions in a one-pot process, employing different temperatures and solvent conditions. 2-methoxyethanol was used as co-solvent to ethanol. The co-solvent ratio and the synthesis temperature were varied. The pore morphology of the materials was characterized by nitrogen porosimetry and small angle neutron scattering (SANS), and the particle morphology by transmission electron microscopy (TEM) and ultra-small angle neutron scattering (USANS). The thermal behavior was investigated by simultaneous thermogravimetry-differential scanning calorimetry (TG-DSC) measurements. The SANS and N₂ sorption results demonstrated that a well-ordered mesoporous structure was obtained at all conditions in the synthesis at room temperature. Addition of methoxyethanol led to an increase of the pore wall thickness. Simultaneously, an increase of methoxyethanol content led to lowering of the mean particle size from 300 to 230 nm, according to the ultra-small angle scattering data. The ordered porosity and high specific surfaces make these materials suitable for applications such as adsorbents in environmental remediation. Batch adsorption measurements of metal ion removal from aqueous solutions of Cu(II) and Pb(II) showed that the materials exhibit dominantly monolayer surface adsorption characteristics. The adsorption capacities were 9.7 mg/g for Cu(II) and 18.8 mg/g for Pb(II) at pH 5, making these materials competitive in performance to various composite materials. Full article

Chemical solution deposition (CSD) of BaTiO₃ (BT) or BT-based thin films relies on using a carboxylic acid and alcohol as the solvents for alkaline-earth carboxylate and transition-metal alkoxide, respectively; however, the esterification reaction of the solvents may lead to in-situ water formation and precipitation. To avoid such an uncontrolled reaction, we developed a route in which ethylene glycol (EG) is used as the solvent for Ba-acetate. The EG-based BT coating solutions are stable for at least a few months. The thermal decomposition of the BT xerogel obtained by drying the EG-based solutions depends on the choice of the solvent for the Ti-alkoxide as well: in the case of EG and 2-methoxyethanol solvents carbon residues are removed at only about 1100 °C, while in the case of ethanol it is concluded at about 700 °C. About 100 nm thick BT films derived from the EG-ethanol solution deposited on platinized silicon reveal dense, crack-free columnar microstructure. They exhibit local ferro- and piezoelectric properties. The macroscopic polarization-electric field loops were obtained up to a quite high electric field of about 2.4 MV/cm. The EG-ethanol based CSD route is a viable alternative to the established acetic acid–alcohol route for BT and BT-based films. Full article

In this paper, undoped, Al-, and In-doped zinc oxide thin films were deposited. Film growth was performed using the sol–gel technique. The method included (a) preparing homogeneous and stable solutions of zinc acetate 2-hydrate, (b) mixing them with aluminum nitrate and indium acetate in 2-methoxyethanol and 2-aminoethanol solutions with various concentrations, and (c) spin coating them onto transparent glass substrates. After thermal annealing, the films showed a high transparency (80–90%) and good stability. Using typical diagnostic tools, the structural, morphological, optical, and electrical film properties were investigated and linked to the dopant type, and concentrations in view of optoelectronics were investigated. Full article

Steroid sapogenin diosgenin is of significant interest due to its biological activity and synthetic application. A consecutive one-pot reaction of diosgenin, oxalyl chloride, arylacetylenes, and phenylhydrazine give rise to steroidal 1,3,5-trisubstituted pyrazoles (isolated yield 46–60%) when the Stephens–Castro reaction and heterocyclization steps were carried out by heating in benzene. When the cyclization step of alkyndione with phenylhydrazine was performed in 2-methoxyethanol at room temperature, steroidal α,β-alkynyl (E)- and (Z)-hydrazones were isolated along with 1,3,5-trisubstituted pyrazole and the isomeric 2,3,5-trisubstituted pyrazole. The consecutive reaction of diosgenin, oxalyl chloride, phenylacetylene and benzoic acid hydrazides efficiently forms steroidal 1-benzoyl-5-hydroxy-3-phenylpyrazolines. The structure of new compounds was unambiguously corroborated by comprehensive NMR spectroscopy, mass-spectrometry, and X-ray structure analyses. Performing the heterocyclization step of ynedione with hydrazine monohydrate in 2-methoxyethanol allowed the synthesis of 5-phenyl substituted steroidal pyrazole, which was found to exhibit high anti-inflammatory activity, comparable to that of diclofenac sodium, a commercial pain reliever. It was shown by molecular docking that the new derivatives are incorporated into the binding site of the protein Keap1 Kelch-domain by their alkynylhydrazone or pyrazole substituent with the formation of more non-covalent bonds and have higher affinity than the initial spirostene core. Full article

The development of selective and robust heterogeneous oxidation catalysts is an enabling technology for conversion of biomass-derived platform chemicals. Vanadium active sites were incorporated into the structure of mesoporous silica via an ultra-fast, one-pot synthesis method based on microwave-assisted heating. In addition, Al/Ti/Zr/Ce anchoring ions were introduced in order to minimize vanadium leaching and better control its dispersion. The supported V-(Al/Ti/Zr/Ce)-MCM-41 composite materials were assessed as catalysts for aerobic C–C bond cleavage of simple models for lignin (1,2-diphenyl-2-methoxyethanol) and sugar-derived polyalcohols (meso-hydrobenzoin). The Ti^IV ions proved to be the best anchors to prevent V leaching, while Al^III and Zr^IV ions were the best to improve selective conversion of the substrates. The active sites in these catalysts are shown to be 2D VO_x layers stabilized on the anchors. In a screen of twelve solvents, weakly polar solvents like toluene were found to be most suitable for this reaction, as was environmentally friendly ethyl acetate. The above properties, together with the high selectivity for C–C bond cleavage, advocate for a heterogeneous catalytic pathway, intrinsically different from that reported previously for molecular oxovanadium (V) catalysts. Full article

The cytotoxicity and microbicidal capacity of seven organic solvents commonly applied for studying plant extracts and bioactive compounds were systematically investigated based on international standards. Four cell lines of normal (CCL-1, HaCaT) or tumor (A-375, A-431) tissue origin, seven bacterial and one fungal strain were used. The impact of the least toxic solvents in the determination of in vitro cytotoxicity was evaluated using a standardized extract from Vaccinium macrocarpon containing 54.2% v/v proanthocyanidins (CystiCran^®). The solvents ethanol, methoxyethanol and polyethylene glycol were the least cytotoxic to all cell lines, with a maximum tolerated concentration (MTC) between 1 and 2% v/v. Ethanol, methanol and polyethylene glycol were mostly suitable for antimicrobial susceptibility testing, with minimum inhibitory concentrations (MICs) ≥ 25% v/v. The MTC values of the solvents dimethyl sulfoxide, dimethoxyethane and dimethylformamide varied from 0.03% to 1.09% v/v. The MICs of dimethyl sulfoxide, methoxyethanol and dimethoxyethane were in the range of 3.125–25% v/v. The cytotoxic effects of CystiCran^® on eukaryotic cell lines were directly proportional to the superimposed effect of the solvents used. The results of this study can be useful for selecting the appropriate solvents for in vitro estimation of the cytotoxic and growth inhibitory effects of bioactive molecules in eukaryotic and prokaryotic cells. Full article

This paper presents the effect of a composite poly(3,4-ethylenedioxythiophene) polystyrene sulfonate PEDOT:PSS and copper-doped nickel oxide (Cu:NiO_x) hole transport layer (HTL) on the performance of perovskite solar cells (PSCs). Thin films of Cu:NiO_x were spin-coated onto fluorine-doped tin oxide (FTO) glass substrates using a blend of nickel acetate tetrahydrate, 2-methoxyethanol and monoethanolamine (MEA) and copper acetate monohydrate. The prepared solution was stirred at 65 °C for 4 h and spin-coated onto the FTO substrates at 3000 rpm for 30 s in a nitrogen glovebox. The Cu:NiOx/FTO/glass structure was then annealed in air at 400 °C for 30 min. A mixture of PEDOT:PSS and isopropyl alcohol (IPA) (in 1:0.05 wt%) was spun onto the Cu:NiO_x/FTO/glass substrate at 4000 rpm for 60 s. The multilayer structure was annealed at 130 °C for 15 min. Subsequently, the perovskite precursor (0.95 M) of methylammonium iodide (MAI) to lead acetate trihydrate (Pb(OAc)₂·3H₂O) was spin-coated at 4000 rpm for 200 s and thermally annealed at 80 °C for 12 min. The inverted planar perovskite solar cells were then fabricated by the deposition of a photoactive layer (CH3NH3PbI3), [6,6]-phenyl C61-butyric acid methyl ester (PCBM), and a Ag electrode. The mechanical behavior of the device during the fabrication of the Cu:NiO_x HTL was modeled with finite element simulations using Abaqus/Complete Abaqus Environment CAE. The results show that incorporating Cu:NiO_x into the PSC device improves its density–voltage (J–V) behavior, giving an enhanced photoconversion efficiency (PCE) of ~12.8% from ~9.8% and ~11.5% when PEDOT:PSS-only and Cu:NiO_x-only are fabricated, respectively. The short circuit current density J_sc for the 0.1 M Cu:NiO_x and 0.2 M Cu:NiO_x-based devices increased by 18% and 9%, respectively, due to the increase in the electrical conductivity of the Cu:NiO_x which provides room for more charges to be extracted out of the absorber layer. The increases in the PCEs were due to the copper-doped nickel oxide blend with the PEDOT:PSS which enhanced the exciton density and charge transport efficiency leading to higher electrical conductivity. The results indicate that the devices with the copper-doped nickel oxide hole transport layer (HTL) are slower to degrade compared with the PEDOT:PSS-only-based HTL. The finite element analyses show that the Cu:NiO_x layer would not extensively deform the device, leading to improved stability and enhanced performance. The implications of the results are discussed for the design of low-temperature solution-processed PSCs with copper-doped nickel oxide composite HTLs. Full article

An [Ru(apy)₂Cl₂] precursor (apy = 2,2′-azopyridine) in 2-methoxyethanol was heated under a pressurized CO atmosphere to afford a diradical complex, [Ru(apy·⁻)₂(CO)₂], containing one-electron-reduced azo anion radical ligands. The electronic states of the complex were characterized by spectroscopic techniques and computational studies. Magnetic measurements revealed the existence of antiferromagnetic interactions in the diradical complex. Full article