N-Heterocyclic carbenes (NHCs) were functionalized with a triisopropylsilyl (TIPS)-protected alkyne group and self-assembled on Au films to enable post-deposition functionalization by C-C coupling reactions. The TIPS group efficiently protected the alkyne and prevented its deprotonation during surface-anchoring of NHC. Sonogashira C-C coupling reactions were performed on the Au film in high yield following removal of the TIPS group, demonstrating that post-deposition coupling reactions can be employed to widen the chemical scope of surface-anchored NHCs.The synthesis and characterization of the adducts of n-alkyl amine and palladium n-alkyl carboxylate, [Pd(R2NH2)2(R1COO)2] (R1 = 1, 7, and 11; R2 = 8, 12, and 16), as precursors for the synthesis of palladium nanoparticles (PdNPs) was carried out via differential scanning calorimetry, FT-IR, Raman and UV-Vis spectroscopy, NMR spectroscopy (1H, 13C pulsed field gradient spin-echo (PGSE), and 13C CP-MAS), and powder X-ray diffraction. Pd n-alkyl carboxylates were obtained by a ligand exchange reaction from palladium acetate and the appropriate aliphatic carboxylic acid. It is proposed that carboxyl moieties in the presence of amine ligands are bound to palladium ions via monodentate bonding as opposed to bridging bidentate coordination of pure palladium carboxylate which exists in the form of polymer aggregates. All the studied palladium carboxylate/amine complexes form bilayer lamellar structures and exhibit first-order melting transitions. The evidence presented in this study shows that the phase behavior of bivalent metal carboxylates is mainly controlled by the type of coordination of carboxylate head groups. For n-alkyl carboxylates, linear chain type aggregates replace the trimeric units of Pd acetate. In solution, in the presence of amine, palladium salt aggregates disintegrate and the Pd complex is isolated and stabilized by amine molecules. https://www.selleckchem.com/products/tak-861.html Using bis(amine) palladium carboxylate adducts as precursors, palladium nanoparticles were fabricated. During high temperature thermolysis, the bis(amine) Pd carboxylate complex decomposes to form small sized Pd nanoparticles. Combining NMR techniques with FTIR spectroscopy, it was possible to follow an original stabilization mechanism. PdNPs are stabilized by weakly interacting long chain aliphatic amide and carboxylic acid derived from the palladium precursor.Semiconducting quantum dots (QDs) have potential applications in light-emitting diodes, single-photon sources and quantum computing due to shape-dependent (opto) electronic properties. Atomic resolution 3D-structure determination is important in understanding growth kinetics and improving device performance. 3D-reconstruction of large QDs was reported using characterization techniques like atomic force microscopy, atom probe tomography and tilt series electron tomography, but, still, atomic resolution tomography of QDs, especially those sized below 10 nm, is a challenge. Inline-3D-holography is an emerging and promising technique to perform atomic resolution tomography at low electron doses. In the present study, atomically resolved 3D structures of QDs were reconstructed using inline-3D-holography, implemented on InN QDs ( less then 10 nm) grown on a Si substrate. The residual amorphous glue distorts the exit surface geometry; hence an error correction method was proposed. This is the first experimental evidence of pre-pyramid shaped 3D structure of QDs sized below 10 nm that supports theoretical predictions.Due to mounting evidence of the negative health effects of persistent perfluoroalkyl acids (PFAAs) with long (i.e., >C7) tails, there is a need for convenient systems capable of sensing these contaminants at dilute aqueous concentrations. To address this concern, a thermoresponsive polymeric network composed of poly(N-isopropylacrylamide) copolymerized with fluorinated comonomers was studied to characterize the gel's physical response to fluorosurfactants in solution. Incorporating fluorinated comonomers into the polymer backbone raised their swelling in fluorocontaminant solutions relative to water - gels synthesized with 10.0 mol% 2,2,2-trifluoroethyl acrylate (TFEA) displayed a heightened maximum water-analyte swelling difference of 3761 ± 147% compared to 3201 ± 466% for non-fluorinated gels in the presence of 1 mM tetraethylammonium perfluorooctane sulfonate (TPFOS). The normalized area under the curve for gels with 12.5 mol% TFEA was further raised to 1.77 ± 0.09, indicating a broadened response window for the contaminant, but at the cost of reducing the overall swelling ratio to 3227 ± 166% and elongating the time required to reach swelling equilibrium. Overall, a copolymer fed with 10.7 mol% TFEA was predicted to maximize both the swelling and response window of the polymer toward TPFOS. Equilibration times followed a logarithmic increase as the percentage of comonomer was raised, noting gradual fluorosurfactant penetration into the gels impeded by initial gel compaction caused by the addition of fluorinated comonomers. Comparative study of gels containing 1H,1H,7H-dodecafluoroheptyl acrylate, TFEA, or 1,1,1,3,3,3-hexafluoroisopropyl acrylate identified careful selection of fluorinated comonomers and their feed ratios as useful tools for tailoring the network's swelling response to TPFOS.The effect of high-pressure torsion (HPT) on the corrosion behavior of extruded ZX00 (Mg-0.45wt%Zn-0.45wt%Ca) in phosphate buffered saline solution is investigated. MgCaZn alloys are promising candidates for the use as bioresorbable implant materials and, therefore, are in the focus of current research. To improve their strength, severe plastic deformation, e.g. via the technique of HPT, can be used. Positron lifetime spectroscopy (PLS) is applied as sensitive tool for studying open-volume defects which evolve during HPT processing and subsequent corrosion. The studies were complemented by electrochemical impedance spectroscopy (EIS). In the uncorroded state, grain boundaries are the major type of positron trap as quantitatively analysed by means of diffusion-reaction models for positron trapping and annihilation in fine-grained alloys. Upon corrosion, positronium formation and annihilation indicate larger open-volume structures, such as pores and cracks, in the emerging corrosion product and oxide layers. Both PLS and EIS clearly show that HPT-deformation strongly reduces the resistance against corrosion.
N-Heterocyclic carbenes (NHCs) were functionalized with a triisopropylsilyl (TIPS)-protected alkyne group and self-assembled on Au films to enable post-deposition functionalization by C-C coupling reactions. The TIPS group efficiently protected the alkyne and prevented its deprotonation during surface-anchoring of NHC. Sonogashira C-C coupling reactions were performed on the Au film in high yield following removal of the TIPS group, demonstrating that post-deposition coupling reactions can be employed to widen the chemical scope of surface-anchored NHCs.The synthesis and characterization of the adducts of n-alkyl amine and palladium n-alkyl carboxylate, [Pd(R2NH2)2(R1COO)2] (R1 = 1, 7, and 11; R2 = 8, 12, and 16), as precursors for the synthesis of palladium nanoparticles (PdNPs) was carried out via differential scanning calorimetry, FT-IR, Raman and UV-Vis spectroscopy, NMR spectroscopy (1H, 13C pulsed field gradient spin-echo (PGSE), and 13C CP-MAS), and powder X-ray diffraction. Pd n-alkyl carboxylates were obtained by a ligand exchange reaction from palladium acetate and the appropriate aliphatic carboxylic acid. It is proposed that carboxyl moieties in the presence of amine ligands are bound to palladium ions via monodentate bonding as opposed to bridging bidentate coordination of pure palladium carboxylate which exists in the form of polymer aggregates. All the studied palladium carboxylate/amine complexes form bilayer lamellar structures and exhibit first-order melting transitions. The evidence presented in this study shows that the phase behavior of bivalent metal carboxylates is mainly controlled by the type of coordination of carboxylate head groups. For n-alkyl carboxylates, linear chain type aggregates replace the trimeric units of Pd acetate. In solution, in the presence of amine, palladium salt aggregates disintegrate and the Pd complex is isolated and stabilized by amine molecules. https://www.selleckchem.com/products/tak-861.html Using bis(amine) palladium carboxylate adducts as precursors, palladium nanoparticles were fabricated. During high temperature thermolysis, the bis(amine) Pd carboxylate complex decomposes to form small sized Pd nanoparticles. Combining NMR techniques with FTIR spectroscopy, it was possible to follow an original stabilization mechanism. PdNPs are stabilized by weakly interacting long chain aliphatic amide and carboxylic acid derived from the palladium precursor.Semiconducting quantum dots (QDs) have potential applications in light-emitting diodes, single-photon sources and quantum computing due to shape-dependent (opto) electronic properties. Atomic resolution 3D-structure determination is important in understanding growth kinetics and improving device performance. 3D-reconstruction of large QDs was reported using characterization techniques like atomic force microscopy, atom probe tomography and tilt series electron tomography, but, still, atomic resolution tomography of QDs, especially those sized below 10 nm, is a challenge. Inline-3D-holography is an emerging and promising technique to perform atomic resolution tomography at low electron doses. In the present study, atomically resolved 3D structures of QDs were reconstructed using inline-3D-holography, implemented on InN QDs ( less then 10 nm) grown on a Si substrate. The residual amorphous glue distorts the exit surface geometry; hence an error correction method was proposed. This is the first experimental evidence of pre-pyramid shaped 3D structure of QDs sized below 10 nm that supports theoretical predictions.Due to mounting evidence of the negative health effects of persistent perfluoroalkyl acids (PFAAs) with long (i.e., >C7) tails, there is a need for convenient systems capable of sensing these contaminants at dilute aqueous concentrations. To address this concern, a thermoresponsive polymeric network composed of poly(N-isopropylacrylamide) copolymerized with fluorinated comonomers was studied to characterize the gel's physical response to fluorosurfactants in solution. Incorporating fluorinated comonomers into the polymer backbone raised their swelling in fluorocontaminant solutions relative to water - gels synthesized with 10.0 mol% 2,2,2-trifluoroethyl acrylate (TFEA) displayed a heightened maximum water-analyte swelling difference of 3761 ± 147% compared to 3201 ± 466% for non-fluorinated gels in the presence of 1 mM tetraethylammonium perfluorooctane sulfonate (TPFOS). The normalized area under the curve for gels with 12.5 mol% TFEA was further raised to 1.77 ± 0.09, indicating a broadened response window for the contaminant, but at the cost of reducing the overall swelling ratio to 3227 ± 166% and elongating the time required to reach swelling equilibrium. Overall, a copolymer fed with 10.7 mol% TFEA was predicted to maximize both the swelling and response window of the polymer toward TPFOS. Equilibration times followed a logarithmic increase as the percentage of comonomer was raised, noting gradual fluorosurfactant penetration into the gels impeded by initial gel compaction caused by the addition of fluorinated comonomers. Comparative study of gels containing 1H,1H,7H-dodecafluoroheptyl acrylate, TFEA, or 1,1,1,3,3,3-hexafluoroisopropyl acrylate identified careful selection of fluorinated comonomers and their feed ratios as useful tools for tailoring the network's swelling response to TPFOS.The effect of high-pressure torsion (HPT) on the corrosion behavior of extruded ZX00 (Mg-0.45wt%Zn-0.45wt%Ca) in phosphate buffered saline solution is investigated. MgCaZn alloys are promising candidates for the use as bioresorbable implant materials and, therefore, are in the focus of current research. To improve their strength, severe plastic deformation, e.g. via the technique of HPT, can be used. Positron lifetime spectroscopy (PLS) is applied as sensitive tool for studying open-volume defects which evolve during HPT processing and subsequent corrosion. The studies were complemented by electrochemical impedance spectroscopy (EIS). In the uncorroded state, grain boundaries are the major type of positron trap as quantitatively analysed by means of diffusion-reaction models for positron trapping and annihilation in fine-grained alloys. Upon corrosion, positronium formation and annihilation indicate larger open-volume structures, such as pores and cracks, in the emerging corrosion product and oxide layers. Both PLS and EIS clearly show that HPT-deformation strongly reduces the resistance against corrosion.
0 Comentários
0 Compartilhamentos
113 Visualizações
0 Anterior
