In the present work ternary composite InBiS3-In2S3-Bi2S3 (IBS) thin films are developed using a homogeneous mixture of precursors [Bi(S2CN(C2H5)2)3]2 (1) and [In(S2CNCy2)3]‧2py (2), separately in toluene and chloroform solutions at 500°C under an inert atmosphere of argon gas via aerosol assisted chemical vapor deposition (AACVD) technique. The phase purity, chemical composition and morphological study of both the films deposited from toluene and chloroform solutions are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy and Field emission scanning electron microscopy (FESEM). The surface morphology showed rod like structure of the films developed from toluene while the films grown from chloroform solution give flake like shapes. The UV-visible spectroscopy explicated that the thin films developed from toluene and chloroform solutions show wide range absorption in whole visible region. Linear Scan voltammetry results show that both the films give negligible dark current, however, the films fabricated from toluene solution give a sharp steep curve with maximum photocurrent density of 2.3 mA‧cm-2 at 0.75 V vs Ag/AgCl/3M KCl using 0.05 M sodium sulphide solution under AM 1.5 G illumination (100 mW‧cm-2), while the film grown from chloroform generates a photocurrent density of 2.1 mA‧cm-2 under similar conditions. The LSV outcomes are further supported by electrochemical impedance spectroscopy (EIS) that gives charge transfer resistance (Rct) value of 8,571 Ω for the films developed from toluene as compared to films fabricated from chloroform with Rct value of 12,476 Ω.
Dithiocarbamate complexes [Cd(S2CNCy2)2(py)] (1), [In(S2CNCy2)3]·2py (2) and [Zn(S2CNCy2)2(py)] (3) were synthesized and toluene solution of (1) and (2) was used as dual source precursor for the synthesis of CdIn2S4 (CIS), while that of (1) and (3) was applied for the deposition of Cd7.23Zn2.77S10–ZnS composite (CZS-ZS) thin film photoan-odes by employing single step aerosol assisted chemical vapor deposition (AACVD) technique. Deposition experiments were performed at 500°C under an inert ambient of argon gas. The structural properties of deposited films were evaluated by using X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The field emission scanning electron microscopy (FESEM) exposed surface morphologies while UV-Visible spectrophotometry revealed that CIS is low band gap photoanode in comparison to CZS-ZS. The comparison of photoelectrochemical (PEC) responses measured in identical conditions in terms of linear sweep voltammetry (LSV) depicts photocurrent density of 4.4 mA /cm2 and 2.9 mA/cm2 at applied potential of 0.7 V under solar light intensity of 100 mW/cm2 for CIS and CZS-ZS respectively. Further, electrochemical impedance spectroscopy (EIS) confirms that PEC properties of CIS are superior to CZS-ZS photoanode as the former offer less charge transfer resistance (Rct) 0.03 MΩ in comparison to CZS-ZS having Rct value of 0.06 MΩ.
Polyolefins have traditionally been polymerized via the heterogeneous Ziegler Natta (Z‐N) catalysts since their discovery in the 1950s, but the later developments of the homogeneous single site metallocene/methylaluminoxane (MAO) catalysts have opened the possibility for the synthesis of polyolefin polymers and copolymers (commercialized in the 1990s) with highly defined microstructure and great degree of control of their molecular architecture resulting in some unique beneficial properties compared to their Z‐N counterparts. The main aim of the work reported here was to examine critically the effects of the processing conditions during multipass extrusions on the molecular and rheological characteristics of metallocene‐catalyzed linear low density polyethylene and a Ziegler‐Natta‐based counterpart polymer and on the thermoxidative (in the melt) stability of their melts and their stabilization. Both polymers examined here were based on ethylene‐1‐hexene copolymers and produced by the same manufacturer with similar density and melt index (MI) values. The melt stability and rheological properties of the polymers were determined from melt flow and capillary rheometric measurements. The molecular characteristics were investigated using GPC for molecular weight determination, 13C‐NMR for short chain branching, 1H‐NMR and FTIR for the type and concentration of unsaturation groups, FTIR for carbonyl‐containing compounds and chemical analysis for hydroperoxide determination. The processibility of the two polymers was compared through examination of different processing conditions (die temperatures 210–285°C, screw speeds 50–200 rpm) used for a multipass extrusion process. Further, the effects of the processing conditions on the melt thermoxidation of the differently catalyzed LLDPE polymers were investigated. The results demonstrated that both the catalyst type and the processing conditions have a great effect on both the rheological and the themoxidative behavior of the polymers as well as on the balance between the competing oxidative reactions taking place in the polymer melt, for example, chain scission and crosslinking reactions. The results obtained for the different multipass extrusion conditions of the two polymers have illustrated clearly that the degradation mechanisms during their melt processing are substantially different. The melt degradation route of the Ziegler‐catalyzed polymer was shown to be dominated by chain scission reactions under all the processing conditions examined, and more so at the higher shear rates and temperatures. By contrast, the evidence clearly showed that the metallocene‐catalyzed polymer gave rise to crosslinking reactions that predominated even under the more severe processing conditions, that is, higher temperatures and shear rates.
Thin films of thallium sulphide (Tl2S) were grown on the FTO surface at three different temperatures (500°C, 550°C, and 600°C) using the aerosol-assisted chemical vapor deposition approach. A thallium diethyldithiocarbamate (Tl[CNS2(C2H5)3]) complex was used as a single-source precursor in tetrahydrofuran (THF) solvent under an inert atmosphere of argon in all deposition experiments. The impact of deposition temperature on structural, morphological, and optical properties of Tl2S thin films was explored using different experimental techniques such as X-ray diffraction (XRD), field-emission scanning electron (FESEM) microscopy, and UV-visible spectrophotometry. XRD analysis specifies that crystallite size varies from 120 to 90 nm with the increase in temperature from 500°C to 600°C. FESEM results revealed that Tl2S films were grown as hexagonal, petals, and marigold flower-like particles at 500°C, 550°C, and 600°C, respectively. UV-visible spectrophotometric analysis shows a decrease in band gap energies with temperature: 1.92 eV at 500°C, 1.72 eV at 550°C, and 1.42 eV at 600°C. The photoelectrochemical measurement in terms of linear sweep voltammetry confirms that the temperature variation has a significant effect on the photoconversion efficiency of Tl2S thin films, and photocurrent density increases from 0.56 to 0.76 mA·cm−2 when the temperature is increased from 500°C to 600°C.
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