A Three‐Step Method for the Deposition of Large Cuboids of Organic–Inorganic Perovskite and Application in Solar Cells

A three‐step method for the deposition of CH₃NH₃PbI₃ perovskite films with a high crystalline structure and large cuboid overlayer morphology is reported. The method includes PbI₂ deposition, which is followed by dipping into a solution of C₄H₉NH₃I (BAI) and (BA)₂PbI₄ perovskite formation. In the final step, the poorly thermodynamically stable (BA)₂PbI₄ phase converts into the more stable CH₃NH₃PbI₃ perovskite by dipping into a solution of CH₃NH₃I. The final product is characterized by XRD, SEM, UV/Vis, and photoluminescence analysis methods. The experimental results indicate that the prepared perovskite has cuboids with high crystallinity and large sizes (up to 1 μm), as confirmed by XRD and SEM data. Photovoltaic investigations show that the three‐step method results in higher solar cell efficiency (15 % enhancement in efficiency) with a better reproducibility than the conventional two‐step deposition method.     

Combination of solid-phase extraction-hollow fiber for ultra-preconcentration of some triazole pesticides followed by gas chromatography-flame ionization detection

In this study, an extraction and preconcentration technique using solid-phase extraction (SPE) along with hollow fiber (HF) has been developed as an ultra-preconcentration technique for some triazole pesticides in aqueous samples. Triazole pesticides were employed as model compounds to assess the method and were monitored by gas chromatography-flame ionization detection (GC-FID). Initially, an aqueous solution of target analytes was passed through an RP-8 SPE cartridge and then the adsorbed analytes were eluted with μL amounts of toluene. The collected elute was slowly introduced into an HF that had one end blocked. This allowed precipitation inside the lumen and pores of the HF. Finally, the obtained HF was mounted on a home-made solid-phase microextraction syringe and entered into the GC injection port for thermal desorption-GC analysis. The effect of various experimental parameters including injection port temperature, desorption time, state of HF, washing solvent, elution solvent and its volume, sample volume, etc. were investigated for finding the optimum conditions. The calibration graphs were linear in the ranges of 2-1000 ng/mL (penconazole and hexaconazole), 5-1000 ng/mL (tebuconazole), 15-1000 ng/mL (triticonazole) and the detection limits (LODs) ranged from 0.6 to 4.5 ng/mL. The enhancement factors were in the range of 870-950. The relative standard deviations (RSD%) for five repeated experiments (C=250 ng/mL of each pesticide) varied from 4.5 to 8.7%. The relative recoveries obtained for analytes in grape juice samples, spiked with different levels of each pesticide, were in the range of 87-119%.     

Synthesis,Characterization and Solvatochromism Investigation of Mixed Ligand Chelate Copper(II) Complexes with Acetyleacetonate and Three Diamine Ligands

The syntheses of three mixed ligand chelate copper(II) complexes of the type [Cu(L)(acac)(H₂O)]BPh₄ where acac=acetyleacetonate; L=N,N‐dimethyl,N′‐benzylethane‐1,2‐diamine ( L¹ ), N,N‐dimethyl, N′‐2‐methylbenzylethane‐1,2‐diamine ( L² ) or N,N‐dimethyl,N′‐2‐chlorobenzylethane‐1,2‐diamine ( L³ ) are reported and characterized by elemental analyses, spectroscopic and molar conductance measurements. The X‐ray structure of complex 1 shows that the central copper atom is placed in a distorted square pyramidal geometry made by acac and diamine chelate in the base and a H₂O molecule on the apex. The prepared complexes are fairly soluble in a large number of organic solvents and show positive solvatochromism. Calculations of SMLR (stepwise multiple linear regression) method was utilized to find the best model explaining the observed solvatochromic behavior and showed that among different solvent parameters, donor number (DN) is a dominant factor responsible for the shift in the d‐d absorption band of the complexes to the lower wavenumber with increasing its values. The importance of substituent effect in diamine ligand on the spectral and SMLR measurements is also discussed.     

Periodic nanostructures on Si(100) surfaces generated by high-repetition rate sub-15 fs pulsed near-infrared laser light

Nanoscale rifts and ripples at a periodicity of 130 nm were generated on Si(100) surfaces immersed in water using tightly focused 800 nm 12 fs pulsed 85 MHz laser light at subnanojoule pulse energies. At radiant exposure close to the ablation threshold rifts were typically 20-50 nm in width and 70 nm in depth running perpendicular to the laser polarization. On increase of the irradiance, the rifts broadened and formed periodic ripples, whereas at highest exposure, a random nanoporous surface topology emerged. Rift and ripple formation is explained by laser-induced standing surface plasma waves, which result in periodic variation of dissipation and ablation.     

Electrochemical Studies and Selective Detection of Thioridazine Using a Carbon Paste Electrode Modified with ZnS Nanoparticles and Simultaneous Determination of Thioridazine and Olanzapine

A novel ZnS nanoparticle‐modified carbon paste electrode (ZnSNP‐MCPE) was fabricated and used to study the electrooxidation of thioridazine (TR) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The determination conditions, such as accumulation time, pH of solution, and modifier amount were optimized. The mechanism of the electrooxidation process on the surface of the modified electrode was studied electrochemically. A linear range of 0.1–36.0 µM with detection limit of 65.0 nM was obtained for TR. In a mixture containing TR and olanzapine (OLZ), the DPV peaks of two compounds can be well separate from each other with a potential difference of 425 mV. Finally, this method was successfully applied to determinate the TR content in real samples.     

High‐mobility solution‐processed zinc oxide thin films on silicon nitride

A high effective electron mobility of 33 cm² V^–1 s^–1 was achieved in solution‐processed undoped zinc oxide (ZnO) thin films. The introduction of silicon nitride (Si₃N₄) as growth substrate resulted in a mobility improvement by a factor of 2.5 with respect to the commonly used silicon oxide (SiO₂). The solution‐processed ZnO thin films grown on Si₃N₄, prepared by low‐pressure chemical vapor deposition, revealed bigger grain sizes, lower strain and better crystalline quality in comparison to the films grown on thermal SiO₂. These results show that the nucleation and growth mechanisms of solution‐processed films are substrate dependent and affect the final film structure accordingly. The substantial difference in electron mobilities suggests that, in addition to the grain morphology and crystalline structure effects, defect chemistry is a contributing factor that also depends on the particular substrate. In this respect, interface trap densities measured in high‐κ HfO₂/ZnO MOSCAPs were about ten times lower in those fabricated on Si₃N₄ substrates. (© 2014 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)

     

Nano- and micro-structure tin (IV) complexes bearing 4-pyridinecarbacylamidophosphate: Sonochemical synthesis,crystal structure,anti-cholinesterase activity,and docking studies

Two di- and triorganotin (IV) complexes, Sn (CH₃)₂Cl₂(4-PCAPh)₂ ( C ₁ ) and Sn(C₆H₅)₃Cl(4-PCAPh) ( C ₂ ); {4-PCAPh = 4-NC₅H₄C(O)NHP(O)(C₆H₁₂N)₂}, have been synthesized and characterized by elemental analysis, ¹H, ¹³C, ³¹P NMR and IR spectroscopy. The crystal structure of C ₁ has been confirmed by X-ray crystallography, which reveals an octahedral geometry surrounding Sn (IV). Both ligands function in an all-trans conformation, with an N-ligated mode for 4-PCAPh. Also, the complexes were prepared at nano- ( Ć ₁ ) and micro-size ( Ć ₂ ) by the sonochemical process. The role of reaction solvent and the concentration of initial reactants on the size and morphology of particles were studied and the products were characterized by X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM). The activities and mechanism of complexes C ₁ , C ₂ , Ć ₁ , Ć ₂ and their corresponding ligand ( L ) on cholinesterase (ChE) were evaluated using a modified Ellman's method and Lineweaver-Burk plots. Nanosheet Ć ₁ showed the best activity against AChE and BChE with the IC₅₀ values being 73.08 ± 0.12 μM and 122.48 ± 0.69 μM, respectively, and the mixed-type mechanism. Molecular modeling simulation revealed the binding interaction template for Sn (CH₃)₂Cl₂(4-PCAPh)₂ with the ChE.     

Development of green sodium sulfate‐induced solidification of floating organic droplets–dispersive liquid phase microextraction method: Application to extraction of four antidepressants

Sodium sulfate‐induced deep eutectic solvent–based solidification of floating organic droplets–dispersive liquid phase microextraction was developed prior to gas chromatography–mass spectrometry. In this method, a mixture of Na₂SO₄ solution (as phase separation agent and disperser) containing menthol–decanoic acid was rapidly injected into an alkaline aqueous solution containing Na₂SO₄. The solution was placed in an ice bath and the menthol–decanoic acid solvent was solidified on the surface of the solution. Under the optimal conditions, the enrichment factors and extraction recoveries were 122–147 and 74–89%, respectively. Finally, an aliquot of the collected organic phase was removed and mixed with acetonitrile and injected into the separation system. The limits of detection and lower limits of quantification were obtained at the ranges of 13–25 and 24–41 ng L^?1, respectively. The relative standard deviations of the proposed method were ≤11% for intra‐ and inter‐day precisions at four concentrations.     

Novel Phosphoranes Containing Urea Derivatives: Synthesis and Characterization

N-Acetyl-N′-methyl urea or ethyl urea in the presence of an acetylenic ester and a desired phosphine functioned as a NH-acid and added to the triple bond in a chemoselective reaction. One of the obtained products underwent lactonization to the corresponding imidazolidine containing ylide moiety when heated in the presence of a base such as triethyl amine.