13 research outputs found
A Large-Scale Synthesis and Characterization of Quaternary CuIn\u3csub\u3e\u3cem\u3ex\u3c/em\u3e\u3c/sub\u3eGa\u3csub\u3e1â\u3cem\u3ex\u3c/em\u3e\u3c/sub\u3eS\u3csub\u3e2\u3c/sub\u3e Chalcopyrite Nanoparticles via Microwave Batch Reactions
Various quaternary CuInxGa1âxS2 (0 †x †1) chalcopyrite nanoparticles have been prepared from molecular single-source precursors via microwave decomposition. We were able to control the nanoparticle size, phase, stoichiometry, and solubility. Depending on the choice of surface modifiers used, we were able to tune the solubility of the resulting nanoparticles. This method has been used to generate up to 5 g of nanoparticles and up to 150 g from multiple batch reactions with excellent reproducibility. Data from UV-Vis, photoluminescence, X-ray diffraction, TEM, DSC/TGA-MS, and ICP-OES analyses have shown high reproducibility in nanoparticle size, composition, and bandgap
A Large-scale Synthesis and Characterization of Quaternary CuInâGaâââSâ Chalcopyrite Nanoparticles via Microwave Batch Reactions
Various quaternary CuInxGa1-xS2 (0â€xâ€1) chalcopyrite nanoparticles have been prepared from molecular single-source precursors via microwave decomposition. We were able to control the nanoparticle size, phase, stoichiometry, and solubility. Depending on the choice of surface modifiers used, we were able to tune the solubility of the resulting nanoparticles. This method has been used to generate up to 5g of nanoparticles and up to 150g from multiple batch reactions with excellent reproducibility. Data from UV-Vis, photoluminescence, X-ray diffraction, TEM, DSC/TGA-MS, and ICP-OES analyses have shown high reproducibility in nanoparticle size, composition, and bandgap
A High-Yield Synthesis of Chalcopyrite CuIn S
We report high-yield and efficient size-controlled syntheses of Chalcopyrite CuInS2 nanoparticles by decomposing molecular single source precursors (SSPs) via microwave irradiation in the presence of 1,2-ethanedithiol at reaction temperatures as low as 100°C and times as short as 30âminutes. The nanoparticles sizes were 1.8ânm to 10.8ânm as reaction temperatures were varied from 100°C to 200°C with the bandgaps from 2.71âeV to 1.28âeV with good size control and high yields (64%â95%). The resulting nanoparticles were analyzed by XRD, UV-Vis, ICP-OES, XPS, SEM, EDS, and HRTEM. Titration studies by 1H NMR using SSP 1 with 1,2-ethanedithiol and benzyl mercaptan were conducted to elucidate the formation of Chalcopyrite CuInS2 nanoparticles
Synthetic control of the cis/trans geometry of M(cyclam)(CCR)\u3csub\u3e2\u3c/sub\u3e]OTf complexes and photophysics of \u3cem\u3ecis\u3c/em\u3e-Cr(cyclam)(CCCF\u3csub\u3e3\u3c/sub\u3e)\u3csub\u3e2\u3c/sub\u3e]OTf and \u3cem\u3ecis\u3c/em\u3e-Rh(cyclam)(CCCF\u3csub\u3e3\u3c/sub\u3e)\u3csub\u3e2\u3c/sub\u3e]OTf
During the synthesis of alkynyl complexes of the type Cr(cyclam)(CCR)2]OTf from cis-Cr(cyclam)(OTf)2]OTf, a cis to trans isomerization occurs that is dependent on the identity of the ether solvent. The isomerization occurs to a significant extent in THF, yielding greater than 80% of the trans isomer, whereas in diethyl ether this isomerization occurs to a lesser extent. Though some base catalyzed isomerization of the final alkynyl product occurs, the data herein supports that the majority of the isomerization occurs during the triflate to alkynyl ligand exchange. It is also demonstrated that 1,1,1,3,3-pentafluoropropane can be used in place of the more expensive 1,1,1-trifluoropropyne for the syntheses of the trifluoropropynyl complexes, cis/trans-M(cyclam)(CCCF3)2]OTf. The methodologies developed are used to prepare the previously unreported cis-M(cyclam)(CCCF3)2]OTf complexes (where MĂ =Ă Cr3+ and Rh3+). Upon photoexcitation, the Cr3+ complex is emissive (738Ă nm) in room temperature acetonitrile with lifetimes of 24Ă ĂÂŒs and 122Ă ĂÂŒs in air saturated and nitrogen purged solutions respectively. The corresponding Rh3+ complex is non-emissive
CCDC 1020834: Experimental Crystal Structure Determination
An entry from the Cambridge Structural Database, the worldâs repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.,Related Article: Parth U. Thakker, Chivin Sun, Levan Khulordava, Colin D. McMillen, Paul S. Wagenknecht|2014|J.Organomet.Chem.|772-773|107|doi:10.1016/j.jorganchem.2014.08.02
Fabrication and Characterization of Thin Film Solar Cell Made from CuIn075Ga025S2 Wurtzite Nanoparticles
DOE EPSCoR [DE-FG02-04ER46142]; National Science Foundation [NSF CHE-1048714, NSF CHE-108952]CuIn0.75Ga0.25S2 (CIGS) thin film solar cells have been successfully fabricated using CIGS Wurtzite phase nanoparticles for the first time. The structure of the cell is Glass/Mo/CIGS/CdS/ZnO/ZnO:Al/Ag. The light absorption layer is made from CIGS Wurtzite phase nanoparticles that are formed from single-source precursors through a microwave irradiation. The Wurtzite phase nanoparticles were converted to Chalcopyrite phase film through a single-step annealing process in the presence of argon and sulfur at 450 degrees C. The solar cell made from Wurtzite phase nanoparticles showed 1.6% efficiency and 0.42 fill factor
CCDC 964986: Experimental Crystal Structure Determination
Related Article: P. Thakker, R. Aru, C. Sun, W. Pennington, A. Siegfried, E. Marder, P. Wagenknecht|2014|Inorg.Chim.Acta|411|158|doi:10.1016/j.ica.2013.11.036,An entry from the Cambridge Structural Database, the worldâs repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures
CCDC 964987: Experimental Crystal Structure Determination
Related Article: P. Thakker, R. Aru, C. Sun, W. Pennington, A. Siegfried, E. Marder, P. Wagenknecht|2014|Inorg.Chim.Acta|411|158|doi:10.1016/j.ica.2013.11.036,An entry from the Cambridge Structural Database, the worldâs repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures
Synthesis of \u3cem\u3etrans\u3c/em\u3e bis-alkynyl complexes of Co(III) supported by a tetradentate macrocyclic amine: A spectroscopic, structural, and electrochemical analysis of Ï-interactions and electronic communication in the CâĄCâMâCâĄC structural unit
Alkynyl complexes of the type trans-Co(cyclam)(CCR)2]OTf have been prepared and characterized by UV-âVis spectroscopy, 1H NMR, vibrational spectroscopy (infrared and Raman), and cyclic voltammetry. Where appropriate the data is compared to the corresponding Cr(III) and Rh(III) complexes. Though the arylalkynyl ligands have been shown to act as ĂâŹ-donors for the corresponding Cr(III) complexes, vibrational spectroscopy suggests that the ĂâŹ-interactions between the arylalkynyl ligands and Co(III) are quite weak, and that the more electron withdrawing trifluoropropynyl ligand likely behaves as a weak ĂâŹ-acceptor toward Co(III). X-ray crystal structures for trans-Co(cyclam)(CCCF3)2]OTf and trans-Cr(cyclam)(CCCF3)2]OTf are also reported and analysis of the MC and CC bond lengths are consistent with this understanding of the trifluoropropynyl ligand. Cyclic voltammetry of the trans-Co(cyclam)(CCR)2]OTf complexes demonstrates that when R=C6H5 or p-C6H4CH3, the CoIII/II reduction wave is chemically irreversible. However, when R=p-C6H4CF3, p-C6H4CN, or CF3, the CoIII/II reduction wave is chemically reversible. This suggests that the more electron withdrawing alkynyl ligands become ĂâŹ-acceptors toward the reduced form of cobalt. Finally, the ferrocenyl capped trans-M(cyclam)(CCFc)2]OTf complexes (where M=Co(III) and Rh(III)) were prepared and studied. Cyclic voltammetry shows only a single 2eĂąËâ wave for the ferrocenyl termini, indicating little to no electronic communication through the organometallic backbone
Trifluoropropynyl as a surrogate for the cyano ligand and intense, room-temperature, metal-centered emission from its Rh(III) complex
The trifluoropropynyl ligand -CĂąâ°ÂĄCCF(3) was studied as a possible surrogate for the cyano ligand. Complexes of the type trans-M(cyclam)(CĂąâ°ÂĄCCF(3))(2)]OTf (where M = Cr(3+), Co(3+), and Rh(3+); OTf = trifluoromethanesulfonate) were prepared and then characterized by electronic spectroscopy and by cyclic voltammetry for the Co(3+) complex. The UV-vis spectra for all three bear a remarkable similarity to that of the trans-M(cyclam)(CN)(2)(+) cations. The trifluoropropynyl complex of Co(3+) shows electrochemical behavior nearly identical with that of its dicyano analogue. Metal-centered phosphorescence from the Rh(III) complex in room-temperature aqueous solution has a quantum yield of 0.12 and a lifetime of 73 ĂÂŒs, nearly 10 times higher than those of its dicyano analogue