Abstract:Herein, we describe the synthesis and characterization of new ligands, N, and N,N-dipropyl-NЈ-(1-naphthoyl)thiourea (1b), and their complexes with copper, bis[N,N-diethyl-NЈ-(1-naphthoyl)thioureato]Cu II (2a) and bis[N,N-dipropyl-NЈ-(1-naphthoyl)thioureato]Cu II (2b). All four compounds (i.e., 1a, 1b, 2a, and 2b) were characterized by elemental analysis, 1 H NMR and 13 C NMR spectroscopy, and FTIR spectroscopy. The structures of compounds 1a, 1b, and 2b were determined by single-crystal X-ray diffraction anal… Show more
“…only Cu is present), flake-like sheets were observed (Fig. 6 f), which is consistent with a previous report of AACVD decomposition of a bis[N,N-dipropyl-N-(1-naphthoyl)thioureato]copper(II) precursor 67 . Figure 6 Representative SEM images of Cu 2x Sb 2(1−x) S y thin film synthesised by the hot-wall AACVD at 450 °C using various values of x, where x = ( a ) 0, ( b ) 0.2, ( c ) 0.4, ( d ) 0.6, ( e ) 0.8 and ( f ) 1.…”
Copper antimony sulfide (Cu-Sb-S) has recently been proposed as an attractive alternative photovoltaic material due to the earth-abundant and non-toxic nature of the elements, high absorption coefficients and band gaps commensurate with efficient harvesting of solar photonic flux across multiple phases of Cu-Sb-S. These materials are therefore highly desirable and sustainable and scalable deposition techniques to produce them are of interest. In this paper, we demonstrate two facile, low-temperature and inexpensive techniques (solventless thermolysis and aerosol-assisted chemical vapor deposition (AACVD)) for the preparation of binary digenite (Cu1.8S), chalcocite (Cu2S) and stibnite (Sb2S3) and several phases of ternary copper-antimony-sulfide (Cu2xSb2(1−x)Sy, where 0 ≤ x ≤ 1). It was found that by utilising these different techniques and varying the ratio of Cu:Sb, pure phases of ternary chalcostibite (CuSbS2), fematinite (Cu3SbS4) and tetrahedrite (Cu12Sb4S13) can be achieved. Two single-source precursors were investigated for this purpose, namely the diethyldithiocarbamate (DTC) complexes of copper and antimony Cu(DTC)2 and Sb(DTC)3. These were decomposed both individually (to produce binary materials) and combined (to produce ternary materials) at different ratios. From the solventless thermolysis and AACVD methods, either particulate or thin film material was formed, respectively. These materials were then characterised by powder XRD, SEM, EDX and Raman spectroscopies to determine the crystalline phase, material morphology and uniformity of elemental composition. This analysis demonstrated that as the Cu-content increases, the phase of the ternary material changes from chalcostibite (CuSbS2) and fematinite (Cu3SbS4) at a low Cu:Sb ratio to tetrahedrite (Cu12Sb4S13) at a high Cu:Sb ratio.
“…only Cu is present), flake-like sheets were observed (Fig. 6 f), which is consistent with a previous report of AACVD decomposition of a bis[N,N-dipropyl-N-(1-naphthoyl)thioureato]copper(II) precursor 67 . Figure 6 Representative SEM images of Cu 2x Sb 2(1−x) S y thin film synthesised by the hot-wall AACVD at 450 °C using various values of x, where x = ( a ) 0, ( b ) 0.2, ( c ) 0.4, ( d ) 0.6, ( e ) 0.8 and ( f ) 1.…”
Copper antimony sulfide (Cu-Sb-S) has recently been proposed as an attractive alternative photovoltaic material due to the earth-abundant and non-toxic nature of the elements, high absorption coefficients and band gaps commensurate with efficient harvesting of solar photonic flux across multiple phases of Cu-Sb-S. These materials are therefore highly desirable and sustainable and scalable deposition techniques to produce them are of interest. In this paper, we demonstrate two facile, low-temperature and inexpensive techniques (solventless thermolysis and aerosol-assisted chemical vapor deposition (AACVD)) for the preparation of binary digenite (Cu1.8S), chalcocite (Cu2S) and stibnite (Sb2S3) and several phases of ternary copper-antimony-sulfide (Cu2xSb2(1−x)Sy, where 0 ≤ x ≤ 1). It was found that by utilising these different techniques and varying the ratio of Cu:Sb, pure phases of ternary chalcostibite (CuSbS2), fematinite (Cu3SbS4) and tetrahedrite (Cu12Sb4S13) can be achieved. Two single-source precursors were investigated for this purpose, namely the diethyldithiocarbamate (DTC) complexes of copper and antimony Cu(DTC)2 and Sb(DTC)3. These were decomposed both individually (to produce binary materials) and combined (to produce ternary materials) at different ratios. From the solventless thermolysis and AACVD methods, either particulate or thin film material was formed, respectively. These materials were then characterised by powder XRD, SEM, EDX and Raman spectroscopies to determine the crystalline phase, material morphology and uniformity of elemental composition. This analysis demonstrated that as the Cu-content increases, the phase of the ternary material changes from chalcostibite (CuSbS2) and fematinite (Cu3SbS4) at a low Cu:Sb ratio to tetrahedrite (Cu12Sb4S13) at a high Cu:Sb ratio.
“…In this context, thiourea derivatives are widely known to be versatile ligand due to their ability of electronic transportation that arises from rigid p-conjugated systems on resonance structures which have been studied in numerous applications [10][11][12], including in molecular electronics [13,14]. The uniqueness of thiourea derivatives are due to their lone pair of N, S and O atoms which involve in the resonance that leads to electronic delocalization throughout the molecular backbone of conjugated molecular system which lead to the effective electrical conductivity properties [15][16][17].…”
A new type of naphthoyl-thiourea derivative namely N-(5-methylpyridine)-N 0 -(1-naphthoyl) thiourea (NT) was successfully synthesized prior to form conductive layer in organic light emitting diode (OLED). The structure of compound was determined via single crystal X-ray crystallography analysis and spectroscopically characterized by infrared spectroscopy, 1 H and 13 C nuclear magnetic resonance, UV-Vis, UV-fluorescence, cyclic voltammetry analysis as well evaluated theoretically via Gaussian 09 software employing DFT approach with set of basis function B3LYP/6-31G (d,p). In turn, the compound was deposited onto ITO substrate through electrochemical deposition method prior the electrical conductivity and performance as OLED was investigated via Four Point Probe and Two Point Probe. From the crystal structure, NT crystallizes as triclinic crystal system in P-1 space group, unit cell parameters a = 7.4916(5) Å , b = 9.4050(7) Å , c = 12.0584(9) Å , a = 69.685 (7)°, b = 82.130 (6)°and c = 71.917 (7)°. The conductivity analysis of NT performed better and exhibited semiconductor material; 0.231 Scm -1 under dark condition which indicates this single molecular system can act as potential OLEDs.Graphical Abstract This contribution reports on the design, preparation, and characterization of new type of naphthoyl-thiourea derivative namely N-(5-methylpyridine)-N 0 -(1-naphthoyl) thiourea (NT) prior acting as potential Organic Light Emitting Diode (OLED).
“…[2] Generally dual source route (DSR) is used for the fabrication of thin films but this approach has the disadvantages of impure films, uncontrolled stoichiometry, and low yields due to multiple steps and involvement of hazardous chemicals. To overcome these disadvantages single source molecular precursors (SMP) have recently gained importance for the fabrication of oxides, sulfides, [3] selenides, [4] and tellurides. [5] SMP approach is advantageous because of good control on stoichiometry, flow, temperature, leak control, and simple installation with safer experimentation.…”
This article presents the synthesis and characterisation (Fourier transform infrared spectroscopy, 1 H NMR and 13 C NMR spectroscopy, CHNS (carbon, hydrogen, nitrogen, sulfur) analysis, atomic absorption spectrometry, and single-crystal X-ray diffraction) of a single source molecular precursor 1-(2-fluorolbenzoyl)-3-(3-ferrocenylphenyl)selenourea (M2F). This precursor has been used for the fabrication of FeSe thin films by aerosol-assisted chemical vapour deposition (AACVD) in the presence of different concentrations of two different surfactants (triton and span) keeping all other conditions the same. Fabricated thin films have been characterised with powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The interaction of the surfactants with the precursor (M2F) has been evaluated with cyclic voltammetry and UV-vis spectroscopy.
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